Plasma assisted surface coating/modification processes - An emerging technology

NASA Technical Reports Server (NTRS)

Spalvins, T.

1987-01-01

A broad understanding of the numerous ion or plasma assisted surface coating/modification processes is sought. An awareness of the principles of these processes is needed before discussing in detail the ion nitriding technology. On the basis of surface modifications arising from ion or plasma energizing and interactions, it can be broadly classified as deposition of distinct overlay coatings (sputtering-dc, radio frequency, magnetron, reactive; ion plating-diode, triode) and surface property modification without forming a discrete coating (ion implantation, ion beam mixing, laser beam irradiation, ion nitriding, ion carburizing, plasma oxidation. These techniques offer a great flexibility and are capable in tailoring desirable chemical and structural surface properties independent of the bulk properties.

Plasma assisted surface coating/modification processes: An emerging technology

NASA Technical Reports Server (NTRS)

Spalvins, T.

1986-01-01

A broad understanding of the numerous ion or plasma assisted surface coating/modification processes is sought. An awareness of the principles of these processes is needed before discussing in detail the ion nitriding technology. On the basis of surface modifications arising from ion or plasma energizing and interactions, it can be broadly classified as deposition of distinct overlay coatings (sputtering-dc, radio frequency, magnetron, reactive; ion plating-diode, triode) and surface property modification without forming a discrete coating (ion implantation, ion beam mixing, laser beam irradiation, ion nitriding, ion carburizing, plasma oxidation). These techniques offer a great flexibility and are capable in tailoring desirable chemical and structural surface properties independent of the bulk properties.

Rolling Contact Fatigue Failure Mechanisms of Plasma-Nitrided Ductile Cast Iron

NASA Astrophysics Data System (ADS)

Wollmann, D.; Soares, G. P. P. P.; Grabarski, M. I.; Weigert, N. B.; Escobar, J. A.; Pintaude, G.; Neves, J. C. K.

2017-05-01

Rolling contact fatigue (RCF) of a nitrided ductile cast iron was investigated. Flat washers machined from a pearlitic ductile cast iron bar were quenched and tempered to maximum hardness, ground, polished and divided into four groups: (1) specimens tested as quenched and tempered; (2) specimens plasma-nitrided for 8 h at 400 °C; (3) specimens plasma-nitrided and submitted to a diffusion process for 16 h at 400 °C; and (4) specimens submitted to a second tempering for 24 h at 400 °C. Hardness profiles, phase analyses and residual stress measurements by x-ray diffraction, surface roughness and scanning electron microscopy were applied to characterize the surfaces at each step of this work. Ball-on-flat washer tests were conducted with a maximum contact pressure of 3.6 GPa, under flood lubrication with a SAE 90 API GL-5 oil at 50 °C. Test ending criterion was the occurrence of a spalling. Weibull analysis was used to characterize RCF's lifetime data. Plasma-nitrided specimens exhibited a shorter RCF lifetime than those just quenched and tempered. The effects of nitriding on the mechanical properties and microstructure of the ductile cast iron are discussed in order to explain the shorter endurance of nitrided samples.

Effect of Plasma Nitriding and Nitrocarburizing on HVOF-Sprayed Stainless Steel Coatings

NASA Astrophysics Data System (ADS)

Park, Gayoung; Bae, Gyuyeol; Moon, Kyungil; Lee, Changhee

2013-12-01

In this work, the effects of plasma nitriding (PN) and nitrocarburizing on HVOF-sprayed stainless steel nitride layers were investigated. 316 (austenitic), 17-4PH (precipitation hardening), and 410 (martensitic) stainless steels were plasma-nitrided and nitrocarburized using a N2 + H2 gas mixture and the gas mixture containing C2H2, respectively, at 550 °C. The results showed that the PN and nitrocarburizing produced a relatively thick nitrided layer consisting of a compound layer and an adjacent nitrogen diffusion layer depending on the crystal structures of the HVOF-sprayed stainless steel coatings. Also, the diffusion depth of nitrogen increased when a small amount of C2H2 (plasma nitrocarburizing process) was added. The PN and nitrocarburizing resulted in not only an increase of the surface hardness, but also improvement of the load bearing capacity of the HVOF-sprayed stainless steel coatings because of the formation of CrN, Fe3N, and Fe4N phases. Also, the plasma-nitrocarburized HVOF-sprayed 410 stainless steel had a superior surface microhardness and load bearing capacity due to the formation of Cr23C6 on the surface.

Structure and properties of nitrided surface layer produced on NiTi shape memory alloy by low temperature plasma nitriding

NASA Astrophysics Data System (ADS)

Czarnowska, Elżbieta; Borowski, Tomasz; Sowińska, Agnieszka; Lelątko, Józef; Oleksiak, Justyna; Kamiński, Janusz; Tarnowski, Michał; Wierzchoń, Tadeusz

2015-04-01

NiTi shape memory alloys are used for bone and cardiological implants. However, on account of the metallosis effect, i.e. the release of the alloy elements into surrounding tissues, they are subjected to various surface treatment processes in order to improve their corrosion resistance and biocompatibility without influencing the required shape memory properties. In this paper, the microstructure, topography and morphology of TiN surface layer on NiTi alloy, and corrosion resistance, both before and after nitriding in low-temperature plasma at 290 °C, are presented. Examinations with the use of the potentiodynamic and electrochemical impedance spectroscopy methods were carried out and show an increase of corrosion resistance in Ringer's solution after glow-discharge nitriding. This surface titanium nitride layer also improved the adhesion of platelets and the proliferation of osteoblasts, which was investigated in in vitro experiments with human cells. Experimental data revealed that nitriding NiTi shape memory alloy under low-temperature plasma improves its properties for bone implant applications.

Single photon emission from plasma treated 2D hexagonal boron nitride.

PubMed

Xu, Zai-Quan; Elbadawi, Christopher; Tran, Toan Trong; Kianinia, Mehran; Li, Xiuling; Liu, Daobin; Hoffman, Timothy B; Nguyen, Minh; Kim, Sejeong; Edgar, James H; Wu, Xiaojun; Song, Li; Ali, Sajid; Ford, Mike; Toth, Milos; Aharonovich, Igor

2018-05-03

Artificial atomic systems in solids are becoming increasingly important building blocks in quantum information processing and scalable quantum nanophotonic networks. Amongst numerous candidates, 2D hexagonal boron nitride has recently emerged as a promising platform hosting single photon emitters. Here, we report a number of robust plasma and thermal annealing methods for fabrication of emitters in tape-exfoliated hexagonal boron nitride (hBN) crystals. A two-step process comprising Ar plasma etching and subsequent annealing in Ar is highly robust, and yields an eight-fold increase in the concentration of emitters in hBN. The initial plasma-etching step generates emitters that suffer from blinking and bleaching, whereas the two-step process yields emitters that are photostable at room temperature with emission wavelengths greater than ∼700 nm. Density functional theory modeling suggests that the emitters might be associated with defect complexes that contain oxygen. This is further confirmed by generating the emitters via annealing hBN in air. Our findings advance the present understanding of the structure of quantum emitters in hBN and enhance the nanofabrication toolkit needed to realize integrated quantum nanophotonic circuits.

Thermal Plasma Synthesis of Crystalline Gallium Nitride Nanopowder from Gallium Nitrate Hydrate and Melamine

PubMed Central

Kim, Tae-Hee; Choi, Sooseok; Park, Dong-Wha

2016-01-01

Gallium nitride (GaN) nanopowder used as a blue fluorescent material was synthesized by using a direct current (DC) non-transferred arc plasma. Gallium nitrate hydrate (Ga(NO3)3∙xH2O) was used as a raw material and NH3 gas was used as a nitridation source. Additionally, melamine (C3H6N6) powder was injected into the plasma flame to prevent the oxidation of gallium to gallium oxide (Ga2O3). Argon thermal plasma was applied to synthesize GaN nanopowder. The synthesized GaN nanopowder by thermal plasma has low crystallinity and purity. It was improved to relatively high crystallinity and purity by annealing. The crystallinity is enhanced by the thermal treatment and the purity was increased by the elimination of residual C3H6N6. The combined process of thermal plasma and annealing was appropriate for synthesizing crystalline GaN nanopowder. The annealing process after the plasma synthesis of GaN nanopowder eliminated residual contamination and enhanced the crystallinity of GaN nanopowder. As a result, crystalline GaN nanopowder which has an average particle size of 30 nm was synthesized by the combination of thermal plasma treatment and annealing. PMID:28344295

Reaction pathways in remote plasma nitridation of ultrathin SiO2 films

NASA Astrophysics Data System (ADS)

Niimi, Hiro; Khandelwal, Amit; Lamb, H. Henry; Lucovsky, Gerald

2002-01-01

Low-temperature nitridation of 3 nm SiO2 films using He/N2 and N2 remote radio frequency (rf) plasmas was investigated. On-line Auger electron spectroscopy and angle-resolved x-ray photoelectron spectroscopy (ARXPS) were employed to determine the concentration, spatial distribution, and local chemical bonding of nitrogen in the resultant films. Experiments were performed using a substrate temperature of 300 °C and 30 W rf power. Nitridation using an upstream He/N2 remote plasma at 0.1 Torr incorporates nitrogen at the top surface of the SiO2 film. In contrast, a lower concentration of nitrogen distributed throughout the film is obtained when the process pressure is increased to 0.3 Torr. ARXPS indicates a N-Si3 local bonding configuration, irrespective of the spatial distribution of N atoms. Slightly more nitrogen is incorporated using a downstream He/N2 plasma at each process pressure. By comparison, nitridation of SiO2 films using a N2 remote plasma at 0.1 Torr is very slow. Optical emission spectroscopy indicates that He dilution enhances the generation of N2+(B 2Σu+) species by altering the plasma electron energy distribution and by providing an additional kinetic pathway (Penning ionization). Changing the He/N2 remote plasma configuration from upstream to downstream (at 0.1 and 0.3 Torr) also enhances N2+(B 2Σu+) generation. For upstream He/N2 remote plasmas, the intensity of N2 first positive emission from N2(B 3Πg) states increases with pressure, whereas the N2+ first negative emission from N2+(B 2Σu+) states decreases. We infer from these observations that N2+ species are primarily responsible for top surface nitridation at 0.1 Torr, and that neutral species [N2(A 3Σu+) metastables and N atoms] are associated with sub-surface nitrogen incorporation.

Surface modification of 17-4PH stainless steel by DC plasma nitriding and titanium nitride film duplex treatment

NASA Astrophysics Data System (ADS)

Qi, F.; Leng, Y. X.; Huang, N.; Bai, B.; Zhang, P. Ch.

2007-04-01

17-4PH stainless steel was modified by direct current (DC) plasma nitriding and titanium nitride film duplex treatment in this study. The microstructure, wear resistance and corrosion resistance were characterized by X-ray diffraction (XRD), pin-on-disk tribological test and polarization experiment. The results revealed that the DC plasma nitriding pretreatment was in favor of improving properties of titanium nitride film. The corrosion resistance and wear resistance of duplex treatment specimen was more superior to that of only coated titanium nitride film.

Photodetectors using III-V nitrides

DOEpatents

Moustakas, T.D.; Misra, M.

1997-10-14

A photodetector using a III-V nitride and having predetermined electrical properties is disclosed. The photodetector includes a substrate with interdigitated electrodes formed on its surface. The substrate has a sapphire base layer, a buffer layer formed from a III-V nitride and a single crystal III-V nitride film. The three layers are formed by electron cyclotron resonance microwave plasma-assisted molecular beam epitaxy (ECR-assisted MBE). Use of the ECR-assisted MBE process allows control and predetermination of the electrical properties of the photodetector. 24 figs.

Photodetectors using III-V nitrides

DOEpatents

Moustakas, Theodore D.; Misra, Mira

1997-01-01

A photodetector using a III-V nitride and having predetermined electrical properties is disclosed. The photodetector includes a substrate with interdigitated electrodes formed on its surface. The substrate has a sapphire base layer, a buffer layer formed from a III-V nitride and a single crystal III-V nitride film. The three layers are formed by electron cyclotron resonance microwave plasma-assisted molecular beam epitaxy (ECR-assisted MBE). Use of the ECR-assisted MBE process allows control and predetermination of the electrical properties of the photodetector.

Low-temperature preparation of GaN-SiO2 interfaces with low defect density. II. Remote plasma-assisted oxidation of GaN and nitrogen incorporation

NASA Astrophysics Data System (ADS)

Bae, Choelhwyi; Lucovsky, Gerald

2004-11-01

Low-temperature remote plasma-assisted oxidation and nitridation processes for interface formation and passivation have been extended from Si and SiC to GaN. The initial oxidation kinetics and chemical composition of thin interfacial oxide were determined from analysis of on-line Auger electron spectroscopy features associated with Ga, N, and O. The plasma-assisted oxidation process is self-limiting with power-law kinetics similar to those for the plasma-assisted oxidation of Si and SiC. Oxidation using O2/He plasma forms nearly pure GaOx, and oxidation using 1% N2O in N2 forms GaOxNy with small nitrogen content, ~4-7 at. %. The interface and dielectric layer quality was investigated using fabricated GaN metal-oxide-semiconductor capacitors. The lowest density of interface states was achieved with a two-step plasma-assisted oxidation and nitridation process before SiO2 deposition.

The Influence of Hot-Rolled Temperature on Plasma Nitriding Behavior of Iron-Based Alloys

NASA Astrophysics Data System (ADS)

El-Hossary, F. M.; Khalil, S. M.; Lotfy, Kh.; Kassem, M. A.

2009-07-01

Experiments were performed with an aim of studying the effect of hot-rolled temperature (600 and 900°C) on radio frequency (rf) plasma nitriding of Fe93Ni4Zr3 alloy. Nitriding was carried out for 10 min in a nitrogen atmosphere at a base pressure of 10-2 mbarr. Different continuous plasma processing powers of 300-550 W in steps 50 W or less were applied. Nitrided hot-rolled specimens were characterized by optical microscopy (OM), X-ray diffraction (XRD) and microhardness measurements. The results reveal that the surface of hot-rolled rf plasma nitrided specimens at 600°C is characterized with a fine microstructure as a result of the high nitrogen solubility and diffusivity. Moreover, the hot-rolled treated samples at 600°C exhibit higher microhardness value than the associated values of hot-rolled treated samples at 900°C. The enhancement of microhardness is due to precipitation and predominance of new phases ( γ and ɛ phases). Mainly, this conclusion has been attributed to the high defect densities and small grain sizes of the samples hot-rolled at 600°C. Generally, the refinement of grain size plays a dramatic role in improvement of mechanical properties of tested samples.

Feasibility study of silicon nitride protection of plastic encapsulated semiconductors

NASA Technical Reports Server (NTRS)

Peters, J. W.; Hall, T. C.; Erickson, J. J.; Gebhart, F. L.

1979-01-01

The application of low temperature silicon nitride protective layers on wire bonded integrated circuits mounted on lead frame assemblies is reported. An evaluation of the mechanical and electrical compatibility of both plasma nitride and photochemical silicon nitride (photonitride) passivations (parallel evaluations) of integrated circuits which were then encapsulated in plastic is described. Photonitride passivation is compatible with all wire bonded lead frame assemblies, with or without initial chip passivation. Plasma nitride passivation of lead frame assemblies is possible only if the chip is passivated before lead frame assembly. The survival rate after the environmental test sequence of devices with a coating of plasma nitride on the chip and a coating of either plasma nitride or photonitride over the assembled device is significantly greater than that of devices assembled with no nitride protective coating over either chip or lead frame.

Synthesis of nanowires and nanoparticles of cubic aluminium nitride

NASA Astrophysics Data System (ADS)

Balasubramanian, C.; Godbole, V. P.; Rohatgi, V. K.; Das, A. K.; Bhoraskar, S. V.

2004-03-01

Nanostructures of cubic aluminium nitride were synthesized by DC arc-plasma-induced melting of aluminium in a nitrogen-argon ambient. The material flux ejected from the molten aluminium surface was found to react with nitrogen under highly non-equilibrium conditions and subsequently condense on a water-cooled surface to yield a mixture of nanowires and nanoparticles of crystalline cubic aluminium nitride. Both x-ray diffraction and electron diffraction measurements revealed that the as-synthesized nitrides adopted the cubic phase. Fourier transform infrared spectroscopy was used to understand the bonding configuration. Microstructural features of the synthesized material were best studied by transmission electron microscopy. From these analyses cubic aluminium nitride was found to be the dominating phase for both nanowires and nanoparticles synthesized at low currents. The typical particle size distribution was found to range over 15-80 nm, whereas the wires varied from 30 to 100 nm in diameter and 500 to 700 nm in length, depending upon the process parameters such as arc current and the nitrogen pressure. The reaction products inside the plasma zone were also obtained theoretically by minimization of free energy and the favourable zone temperature necessary for the formation of aluminium nitride was found to be {\\sim } 6000 K. Results are discussed in view of the highly non-equilibrium conditions that prevail during the arc-plasma synthesis.

Temporally and Spatially Resolved Plasma Spectroscopy in Pulsed Laser Deposition of Ultra-Thin Boron Nitride Films (Postprint)

DTIC Science & Technology

2015-04-24

AFRL-RX-WP-JA-2016-0196 TEMPORALLY AND SPATIALLY RESOLVED PLASMA SPECTROSCOPY IN PULSED LASER DEPOSITION OF ULTRA-THIN BORON NITRIDE...AND SPATIALLY RESOLVED PLASMA SPECTROSCOPY IN PULSED LASER DEPOSITION OF ULTRA-THIN BORON NITRIDE FILMS (POSTPRINT) 5a. CONTRACT NUMBER FA8650...distributions within a PVD plasma plume ablated from a boron nitride (BN) target by a KrF laser at different pressures of nitrogen gas were investigated

Isotropic plasma etching of Ge Si and SiN x films

DOE PAGES

Henry, Michael David; Douglas, Erica Ann

2016-08-31

This study reports on selective isotropic dry etching of chemically vapor deposited (CVD) Ge thin film, release layers using a Shibaura chemical downstream etcher (CDE) with NF 3 and Ar based plasma chemistry. Relative etch rates between Ge, Si and SiN x are described with etch rate reductions achieved by adjusting plasma chemistry with O 2. Formation of oxides reducing etch rates were measured for both Ge and Si, but nitrides or oxy-nitrides created using direct injection of NO into the process chamber were measured to increase Si and SiN x etch rates while retarding Ge etching.

Metal surface nitriding by laser induced plasma

NASA Astrophysics Data System (ADS)

Thomann, A. L.; Boulmer-Leborgne, C.; Andreazza-Vignolle, C.; Andreazza, P.; Hermann, J.; Blondiaux, G.

1996-10-01

We study a nitriding technique of metals by means of laser induced plasma. The synthesized layers are composed of a nitrogen concentration gradient over several μm depth, and are expected to be useful for tribological applications with no adhesion problem. The nitriding method is tested on the synthesis of titanium nitride which is a well-known compound, obtained at present by many deposition and diffusion techniques. In the method of interest, a laser beam is focused on a titanium target in a nitrogen atmosphere, leading to the creation of a plasma over the metal surface. In order to understand the layer formation, it is necessary to characterize the plasma as well as the surface that it has been in contact with. Progressive nitrogen incorporation in the titanium lattice and TiN synthesis are studied by characterizing samples prepared with increasing laser shot number (100-4000). The role of the laser wavelength is also inspected by comparing layers obtained with two kinds of pulsed lasers: a transversal-excited-atmospheric-pressure-CO2 laser (λ=10.6 μm) and a XeCl excimer laser (λ=308 nm). Simulations of the target temperature rise under laser irradiation are performed, which evidence differences in the initial laser/material interaction (material heated thickness, heating time duration, etc.) depending on the laser features (wavelength and pulse time duration). Results from plasma characterization also point out that the plasma composition and propagation mode depend on the laser wavelength. Correlation of these results with those obtained from layer analyses shows at first the important role played by the plasma in the nitrogen incorporation. Its presence is necessary and allows N2 dissociation and a better energy coupling with the target. Second, it appears that the nitrogen diffusion governs the nitriding process. The study of the metal nitriding efficiency, depending on the laser used, allows us to explain the differences observed in the layer features as purity, thickness, and surface morphology.

Influence of nitrogen admixture to argon on the ion energy distribution in reactive high power pulsed magnetron sputtering of chromium

NASA Astrophysics Data System (ADS)

Breilmann, W.; Maszl, C.; Hecimovic, A.; von Keudell, A.

2017-04-01

Reactive high power impulse magnetron sputtering (HiPIMS) of metals is of paramount importance for the deposition of various oxides, nitrides and carbides. The addition of a reactive gas such as nitrogen to an argon HiPIMS plasma with a metal target allows the formation of the corresponding metal nitride on the substrate. The addition of a reactive gas introduces new dynamics into the plasma process, such as hysteresis, target poisoning and the rarefaction of two different plasma gases. We investigate the dynamics for the deposition of chromium nitride by a reactive HiPIMS plasma using energy- and time-resolved ion mass spectrometry, fast camera measurements and temporal and spatially resolved optical emission spectroscopy. It is shown that the addition of nitrogen to the argon plasma gas significantly changes the appearance of the localized ionization zones, the so-called spokes, in HiPIMS plasmas. In addition, a very strong modulation of the metal ion flux within each HiPIMS pulse is observed, with the metal ion flux being strongly suppressed and the nitrogen molecular ion flux being strongly enhanced in the high current phase of the pulse. This behavior is explained by a stronger return effect of the sputtered metal ions in the dense plasma above the racetrack. This is best observed in a pure nitrogen plasma, because the ionization zones are mostly confined, implying a very high local plasma density and consequently also an efficient scattering process.

Microstructure and corrosion resistance of nitrogen-rich surface layers on AISI 304 stainless steel by rapid nitriding in a hollow cathode discharge

NASA Astrophysics Data System (ADS)

Li, Yang; He, Yongyong; Zhang, Shangzhou; Wang, Wei; Zhu, Yijie

2018-01-01

Nitriding treatments have been successfully applied to austenitic stainless steels to improve their hardness and tribological properties. However, at temperatures above 450 °C, conventional plasma nitriding processes decrease the corrosion resistance due to the formation of CrN phases within the modified layer. In this work, AISI 304 austenitic stainless steels were efficiently treated by rapid plasma nitriding at a high temperature of 530 °C in a hollow cathode discharge. The enhanced ionization obtained in the hollow cathode configuration provided a high current density and, consequently, a high temperature could be attained in a short time. The nitrided layers were characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy, transmission electron microscopy and X-ray photoelectron spectroscopy. The results indicated that the dual-layer structure of the nitrided layer consists of a high-N face-centered cubic structure with a free CrN precipitate outer (top) layer and a nitrogen-expanded austenite S-phase bottom layer. The rapid nitriding-assisted hollow cathode discharge technique permits the use of high temperatures, as high as 530 °C, without promoting degradation in the corrosion resistance of stainless steel.

Spherical boron nitride particles and method for preparing them

DOEpatents

Phillips, Jonathan; Gleiman, Seth S.; Chen, Chun-Ku

2003-11-25

Spherical and polyhedral particles of boron nitride and method of preparing them. Spherical and polyhedral particles of boron nitride are produced from precursor particles of hexagonal phase boron nitride suspended in an aerosol gas. The aerosol is directed to a microwave plasma torch. The torch generates plasma at atmospheric pressure that includes nitrogen atoms. The presence of nitrogen atoms is critical in allowing boron nitride to melt at atmospheric pressure while avoiding or at least minimizing decomposition. The plasma includes a plasma hot zone, which is a portion of the plasma that has a temperature sufficiently high to melt hexagonal phase boron nitride. In the hot zone, the precursor particles melt to form molten particles that acquire spherical and polyhedral shapes. These molten particles exit the hot zone, cool, and solidify to form solid particles of boron nitride with spherical and polyhedral shapes. The molten particles can also collide and join to form larger molten particles that lead to larger spherical and polyhedral particles.

High-density plasma etching of III-nitrides: Process development, device applications and damage remediation

NASA Astrophysics Data System (ADS)

Singh, Rajwinder

Plasma-assisted etching is a key technology for III-nitride device fabrication. The inevitable etch damage resulting from energetic pattern transfer is a challenge that needs to be addressed in order to optimize device performance and reliability. This dissertation focuses on the development of a high-density inductively-coupled plasma (ICP) etch process for III-nitrides, the demonstration of its applicability to practical device fabrication using a custom built ICP reactor, and development of techniques for remediation of etch damage. A chlorine-based standard dry etch process has been developed and utilized in fabrication of a number of electronic and optoelectronic III-nitride devices. Annealing studies carried out at 700°C have yielded the important insight that the annealing time necessary for making good-quality metal contacts to etch processed n-GaN is very short (<30 sec), comparable with the annealing times necessary for dopant activation of p-GaN films and provides an opportunity for streamlining process flow. Plasma etching degrades contact quality on n-GaN films and this degradation has been found to increase with the rf bias levels (ion energies) used, most notably in films with higher doping levels. Immersion in 1:1 mixture of hydrochloric acid and de-ionized water, prior to metallization, removes some of the etch damage and is helpful in recovering contact quality. In-situ treatment consisting of a slow ramp-down of rf bias at the end of the etch is found to achieve the same effect as the ex-situ treatment. This insitu technique is significantly advantageous in a large-scale production environment because it eliminates a process step, particularly one involving treatment in hydrochloric acid. ICP equipment customization for scaling up the process to full 2-inch wafer size is described. Results on etching of state of the art 256 x 256 AlGaN focal plane arrays of ultraviolet photodetectors are reported, with excellent etch uniformity over the wafer area.

Nanotribological response of a plasma nitrided bio-steel.

PubMed

Samanta, Aniruddha; Chakraborty, Himel; Bhattacharya, Manjima; Ghosh, Jiten; Sreemany, Monjoy; Bysakh, Sandip; Rane, Ramkrishna; Joseph, Alphonsa; Jhala, Ghanshyam; Mukherjee, Subroto; Das, Mitun; Mukhopadhyay, Anoop K

2017-01-01

AISI 316L is a well known biocompatible, austenitic stainless steel (SS). It is thus a bio-steel. Considering its importance as a bio-prosthesis material here we report the plasma nitriding of AISI 316L (SS) followed by its microstructural and nanotribological characterization. Plasma nitriding of the SS samples was carried out in a plasma reactor with a hot wall vacuum chamber. For ease of comparison these plasma nitrided samples were termed as SSPN. The experimental results confirmed the formations of an embedded nitrided metal layer zone (ENMLZ) and an interface zone (IZ) between the ENMLZ and the unnitrided bulk metallic layer zone (BMLZ) in the SSPN sample. These ENMLZ and IZ in the SSPN sample were richer in iron nitride (FeN) chromium nitride (CrN) along with the austenite phase. The results from nanoindentation, microscratch, nanoscratch and sliding wear studies confirmed that the static contact deformation resistance, the microwear, nanowear and sliding wear resistance of the SSPN samples were much better than those of the SS samples. These results were explained in terms of structure-property correlations. Copyright © 2016 Elsevier Ltd. All rights reserved.

Novel Cyclosilazane-Type Silicon Precursor and Two-Step Plasma for Plasma-Enhanced Atomic Layer Deposition of Silicon Nitride.

PubMed

Park, Jae-Min; Jang, Se Jin; Lee, Sang-Ick; Lee, Won-Jun

2018-03-14

We designed cyclosilazane-type silicon precursors and proposed a three-step plasma-enhanced atomic layer deposition (PEALD) process to prepare silicon nitride films with high quality and excellent step coverage. The cyclosilazane-type precursor, 1,3-di-isopropylamino-2,4-dimethylcyclosilazane (CSN-2), has a closed ring structure for good thermal stability and high reactivity. CSN-2 showed thermal stability up to 450 °C and a sufficient vapor pressure of 4 Torr at 60 °C. The energy for the chemisorption of CSN-2 on the undercoordinated silicon nitride surface as calculated by density functional theory method was -7.38 eV. The PEALD process window was between 200 and 500 °C, with a growth rate of 0.43 Å/cycle. The best film quality was obtained at 500 °C, with hydrogen impurity of ∼7 atom %, oxygen impurity less than 2 atom %, low wet etching rate, and excellent step coverage of ∼95%. At 300 °C and lower temperatures, the wet etching rate was high especially at the lower sidewall of the trench pattern. We introduced the three-step PEALD process to improve the film quality and the step coverage on the lower sidewall. The sequence of the three-step PEALD process consists of the CSN-2 feeding step, the NH 3 /N 2 plasma step, and the N 2 plasma step. The H radicals in NH 3 /N 2 plasma efficiently remove the ligands from the precursor, and the N 2 plasma after the NH 3 plasma removes the surface hydrogen atoms to activate the adsorption of the precursor. The films deposited at 300 °C using the novel precursor and the three-step PEALD process showed a significantly improved step coverage of ∼95% and an excellent wet etching resistance at the lower sidewall, which is only twice as high as that of the blanket film prepared by low-pressure chemical vapor deposition.

The effect of surface nanocrystallization on plasma nitriding behaviour of AISI 4140 steel

NASA Astrophysics Data System (ADS)

Li, Yang; Wang, Liang; Zhang, Dandan; Shen, Lie

2010-11-01

A plastic deformation surface layer with nanocrystalline grains was produced on AISI 4140 steel by means of surface mechanical attrition treatment (SMAT). Plasma nitriding of SMAT and un-SMAT AISI 4140 steel was carried out by a low-frequency pulse excited plasma unit. A series of nitriding experiments has been conducted at temperatures ranging from 380 to 500 °C for 8 h in an NH 3 gas. The samples were characterized using X-ray diffraction, scanning electron microscopy, optical microscopy and Vickers microhardness tester. The results showed that a much thicker compound layer with higher hardness was obtained for the SMAT samples when compared with un-SMAT samples after nitriding at the low temperature. In particular, plasma nitriding SMAT AISI 4140 steel at 380 °C for 8 h can produced a compound layer of 2.5 μm thickness with very high hardness on the surface, which is similar to un-SMAT samples were plasma nitrided at approximately 430 °C within the same time.

Reactive Spark Plasma Sintering (SPS) of Nitride Reinforced Titanium Alloy Composites (Postprint)

DTIC Science & Technology

2014-08-15

AFRL-RX-WP-JA-2014-0177 REACTIVE SPARK PLASMA SINTERING (SPS) OF NITRIDE REINFORCED TITANIUM ALLOY COMPOSITES (POSTPRINT) Jaimie S...titanium–vanadium alloys, has been achieved by introducing reactive nitrogen gas during the spark plasma sintering (SPS) of blended titanium and...lcomReactive spark plasma sintering (SPS) of nitride reinforced titanium alloy compositeshttp://dx.doi.org/10.1016/j.jallcom.2014.08.049 0925-8388

Distortion control in 20MnCr5 bevel gears after liquid nitriding process to maintain precision dimensions

NASA Astrophysics Data System (ADS)

Mahendiran, M.; Kavitha, M.

2018-02-01

Robotic and automotive gears are generally very high precision components with limitations in tolerances. Bevel gears are more widely used and dimensionally very close tolerance components that need stability without any backlash or distortion for smooth and trouble free functions. Nitriding is carried out to enhance wear resistance of the surface. The aim of this paper is to reduce the distortion in liquid nitriding process, though plasma nitriding is preferred for high precision components. Various trials were conducted to optimize the process parameters, considering pre dimensional setting for nominal nitriding layer growth. Surface cleaning, suitable fixtures and stress relieving operations were also done to optimize the process. Micro structural analysis and Vickers hardness testing were carried out for analyzing the phase changes, variation in surface hardness and case depth. CNC gear testing machine was used for determining the distortion level. The presence of white layer was found for about 10-15μm in the case depth of 250± 3.5μm showing an average surface hardness of 670 HV. Hence the economical liquid nitriding process was successfully used for producing high hardness and wear resistant coating over 20MnCr5 material with less distortion and reduced secondary grinding process for dimensional control.

Device performance of in situ steam generated gate dielectric nitrided by remote plasma nitridation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Al-Shareef, H. N.; Karamcheti, A.; Luo, T. Y.

2001-06-11

In situ steam generated (ISSG) oxides have recently attracted interest for use as gate dielectrics because of their demonstrated reliability improvement over oxides formed by dry oxidation. [G. Minor, G. Xing, H. S. Joo, E. Sanchez, Y. Yokota, C. Chen, D. Lopes, and A. Balakrishna, Electrochem. Soc. Symp. Proc. 99-10, 3 (1999); T. Y. Luo, H. N. Al-Shareef, G. A. Brown, M. Laughery, V. Watt, A. Karamcheti, M. D. Jackson, and H. R. Huff, Proc. SPIE 4181, 220 (2000).] We show in this letter that nitridation of ISSG oxide using a remote plasma decreases the gate leakage current of ISSGmore » oxide by an order of magnitude without significantly degrading transistor performance. In particular, it is shown that the peak normalized transconductance of n-channel devices with an ISSG oxide gate dielectric decreases by only 4% and the normalized drive current by only 3% after remote plasma nitridation (RPN). In addition, it is shown that the reliability of the ISSG oxide exhibits only a small degradation after RPN. These observations suggest that the ISSG/RPN process holds promise for gate dielectric applications. {copyright} 2001 American Institute of Physics.« less

Defect mediated van der Waals epitaxy of hexagonal boron nitride on graphene

NASA Astrophysics Data System (ADS)

Heilmann, M.; Bashouti, M.; Riechert, H.; Lopes, J. M. J.

2018-04-01

Van der Waals heterostructures comprising of hexagonal boron nitride and graphene are promising building blocks for novel two-dimensional devices such as atomically thin transistors or capacitors. However, demonstrators of those devices have been so far mostly fabricated by mechanical assembly, a non-scalable and time-consuming method, where transfer processes can contaminate the surfaces. Here, we investigate a direct growth process for the fabrication of insulating hexagonal boron nitride on high quality epitaxial graphene using plasma assisted molecular beam epitaxy. Samples were grown at varying temperatures and times and studied using atomic force microscopy, revealing a growth process limited by desorption at high temperatures. Nucleation was mostly commencing from morphological defects in epitaxial graphene, such as step edges or wrinkles. Raman spectroscopy combined with x-ray photoelectron measurements confirm the formation of hexagonal boron nitride and prove the resilience of graphene against the nitrogen plasma used during the growth process. The electrical properties and defects in the heterostructures were studied with high lateral resolution by tunneling current and Kelvin probe force measurements. This correlated approach revealed a nucleation apart from morphological defects in epitaxial graphene, which is mediated by point defects. The presented results help understanding the nucleation and growth behavior during van der Waals epitaxy of 2D materials, and point out a route for a scalable production of van der Waals heterostructures.

Constricted glow discharge plasma source

DOEpatents

Anders, Andre; Anders, Simone; Dickinson, Michael; Rubin, Michael; Newman, Nathan

2000-01-01

A constricted glow discharge chamber and method are disclosed. The polarity and geometry of the constricted glow discharge plasma source is set so that the contamination and energy of the ions discharged from the source are minimized. The several sources can be mounted in parallel and in series to provide a sustained ultra low source of ions in a plasma with contamination below practical detection limits. The source is suitable for applying films of nitrides such as gallium nitride and oxides such as tungsten oxide and for enriching other substances in material surfaces such as oxygen and water vapor, which are difficult process as plasma in any known devices and methods. The source can also be used to assist the deposition of films such as metal films by providing low-energy ions such as argon ions.

Microstructure and dry-sliding wear properties of DC plasma nitrided 17-4 PH stainless steel

NASA Astrophysics Data System (ADS)

Li, Gui-jiang; Wang, Jun; Li, Cong; Peng, Qian; Gao, Jian; Shen, Bao-luo

2008-05-01

An attempt that the precipitation hardening steel 17-4PH was conducted by DC plasma nitriding (DCPN) is made to develop a kind of candidate material for nuclear reactor. Nitriding process performed at temperature ⩽ 400 °C takes effect on creation of the layers composed of S-phase (expanded austenite) and αN‧ (expanded martensite). Up to the temperature of 420 °C, the S-phase peaks disappear due to the transformation occurrence (S-phase → αN‧ + CrN). For the samples nitrided at temperature ⩾ 450 °C, no evidence of αN‧ is found owing to a precipitation (αN‧ → α +CrN) taking place. For the 480 °C/4 h treated sample, it is the surface microhardness that plays the lead role in the wear rate reduction but the surface roughness; while for the 400 °C/4 h treated sample, it is both of the surface roughness and the S-phase formation. Dry sliding wear of the untreated 17-4PH is mainly characterized by strong adhesion, abrasion and oxidation mechanism. Samples nitrided at 400 °C which is dominated by slight abrasion and plastic deformation exhibit the best dry sliding wear resistance compared to the samples nitrided at other temperatures.

Phase formation in selected surface-roughened plasma-nitrided 304 austenite stainless steel.

PubMed

Singh, Gajendra Prasad; Joseph, Alphonsa; Raole, Prakash Manohar; Barhai, Prema Kanta; Mukherjee, Subroto

2008-04-01

Direct current (DC) glow discharge plasma nitriding was carried out on three selected surface-roughened AISI 304 stainless steel samples at 833 K under 4 mbar pressures for 24 h in the presence of N 2 :H 2 gas mixtures of 50 : 50 ratios. After plasma nitriding, the phase formation, case depth, surface roughness, and microhardness of a plasma-nitrided layer were evaluated by glancing angle x-ray diffractogram, optical microscope, stylus profilometer, and Vickers microhardness tester techniques. The case depth, surface hardness, and phase formation variations were observed with a variation in initial surface roughness. The diffraction patterns of the plasma-nitrided samples showed the modified intensities of the α and γ phases along with those of the CrN, Fe 4 N, and Fe 3 N phases. Hardness and case depth variations were observed with a variation in surface roughness. A maximum hardness of 1058 Hv and a case depth of 95 μm were achieved in least surface-roughened samples.

Tribological and corrosion properties of plasma nitrided and nitrocarburized 42CrMo4 steel

NASA Astrophysics Data System (ADS)

Kusmic, D.; Van Thanh, D.

2017-02-01

This article deals with tribological and corrosion resistance comparison of plasma nitrided and nitrocarburized 42CrMo4 steel used for breech mechanism in the armament production. Increasing of materials demands (like wear resistance, surface hardness, running-in properties and corrosion resistance) used for armament production and in other industrial application leads in the field of surface treatment. Experimental steel samples were plasma nitrided under different nitriding gas ratio at 500 °C for 15h and nitrocarburized for 45 min at temperature 590°C and consequently post-oxidized for 10 min at 430°C. Individual 42CrMo4 steel samples were subsequently metallographically evaluated and characterized by hardness and microhardness measuring. The wear test “ball on disc” was realized for measuring of adhesive wear and coefficient of friction during unlubricated sliding. NSS corrosion tests were realized for corrosion resistance evaluation and expressed by corroded area and calculated corrosion rate. The corrosion resistance evaluation is by the surface corrosion-free surfaces evaluation supplemented using the laser confocal microscopy. Due to different surface treatment and plasma nitriding conditions, there are wear resistance and corrosion resistance differences evident between the plasma nitrided steel samples as well.

Nitridation of porous GaAs by an ECR ammonia plasma

NASA Astrophysics Data System (ADS)

Naddaf, M.; Hullavarad, S. S.; Ganesan, V.; Bhoraskar, S. V.

2006-02-01

The effect of surface porosity of GaAs on the nature of growth of GaN, by use of plasma nitridation of GaAs, has been investigated. Porous GaAs samples were prepared by anodic etching of n-type (110) GaAs wafers in HCl solution. Nitridation of porous GaAs samples were carried out by using an electron-cyclotron resonance-induced ammonia plasma. The formation of mixed phases of GaN was investigated using the grazing angle x-ray diffraction method. A remarkable improvement in the intensity of photoluminescence (PL) compared with that of GaN synthesized by direct nitriding of GaAs surface has been observed. The PL intensity of nitrided porous GaAs at the temperature of 380 °C was found to be about two orders of magnitude higher as compared with the directly nitrided GaAs at the temperature of 500 °C. The changes in the morphology of nitrided porous GaAs have been investigated using both scanning electron microscopy and atomic force microscopy.

Method to synthesize bulk iron nitride

DOE Office of Scientific and Technical Information (OSTI.GOV)

Monson, Todd; Lavernia, Enrique J.; Zheng, Baolong

Bulk iron nitride can be synthesized from iron nitride powder by spark plasma sintering. The iron nitride can be spark plasma sintered at a temperature of less than 600°C. and a pressure of less than 600 MPa, with 400 MPa or less most often being sufficient. High pressure SPS can consolidate dense iron nitrides at a lower temperature to avoid decomposition. The higher pressure and lower temperature of spark discharge sintering avoids decomposition and limits grain growth, enabling enhanced magnetic properties. The method can further comprise synthesis of nanocrystalline iron nitride powders using two-step reactive milling prior to high-pressure sparkmore » discharge sintering.« less

Surface reaction of silicon chlorides during atomic layer deposition of silicon nitride

NASA Astrophysics Data System (ADS)

Yusup, Luchana L.; Park, Jae-Min; Mayangsari, Tirta R.; Kwon, Young-Kyun; Lee, Won-Jun

2018-02-01

The reaction of precursor with surface active site is the critical step in atomic layer deposition (ALD) process. We performed the density functional theory calculation with DFT-D correction to study the surface reaction of different silicon chloride precursors during the first half cycle of ALD process. SiCl4, SiH2Cl2, Si2Cl6 and Si3Cl8 were considered as the silicon precursors, and an NH/SiNH2*-terminated silicon nitride surface was constructed to model the thermal ALD processes using NH3 as well as the PEALD processes using NH3 plasma. The total energies of the system were calculated for the geometry-optimized structures of physisorption, chemisorption, and transition state. The order of silicon precursors in energy barrier, from lowest to highest, is Si3Cl8 (0.92 eV), Si2Cl6 (3.22 eV), SiH2Cl2 (3.93 eV) and SiCl4 (4.49 eV). Silicon precursor with lower energy barrier in DFT calculation showed lower saturation dose in literature for both thermal and plasma-enhanced ALD of silicon nitride. Therefore, DFT calculation is a promising tool in predicting the reactivity of precursor during ALD process.

Adhesion, friction, and wear of plasma-deposited thin silicon nitride films at temperatures to 700 C

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Pouch, J. J.; Alterovitz, S. A.; Pantic, D. M.; Johnson, G. A.

1988-01-01

The adhesion, friction, and wear behavior of silicon nitride films deposited by low- and high-frequency plasmas (30 kHz and 13.56 MHz) at various temperatures to 700 C in vacuum were examined. The results of the investigation indicated that the Si/N ratios were much greater for the films deposited at 13.56 MHz than for those deposited at 30 kHz. Amorphous silicon was present in both low- and high-frequency plasma-deposited silicon nitride films. However, more amorphous silicon occurred in the films deposited at 13.56 MHz than in those deposited at 30 kHz. Temperature significantly influenced adhesion, friction, and wear of the silicon nitride films. Wear occurred in the contact area at high temperature. The wear correlated with the increase in adhesion and friction for the low- and high-frequency plasma-deposited films above 600 and 500 C, respectively. The low- and high-frequency plasma-deposited thin silicon nitride films exhibited a capability for lubrication (low adhesion and friction) in vacuum at temperatures to 500 and 400 C, respectively.

Combined angle-resolved X-ray photoelectron spectroscopy, density functional theory and kinetic study of nitridation of gallium arsenide

NASA Astrophysics Data System (ADS)

Mehdi, H.; Monier, G.; Hoggan, P. E.; Bideux, L.; Robert-Goumet, C.; Dubrovskii, V. G.

2018-01-01

The high density of interface and surface states that cause the strong Fermi pinning observed on GaAs surfaces can be reduced by depositing GaN ultra-thin films on GaAs. To further improve this passivation, it is necessary to investigate the nitridation phenomena by identifying the distinct steps occurring during the process and to understand and quantify the growth kinetics of GaAs nitridation under different conditions. Nitridation of the cleaned GaAs substrate was performed using N2 plasma source. Two approaches have been combined. Firstly, an AR-XPS (Angle Resolved X-ray Photoelectron Spectroscopy) study is carried out to determine the chemical environments of the Ga, As and N atoms and the composition depth profile of the GaN thin film which allow us to summarize the nitridation process in three steps. Moreover, the temperature and time treatment have been investigated and show a significant impact on the formation of the GaN layer. The second approach is a refined growth kinetic model which better describes the GaN growth as a function of the nitridation time. This model clarifies the exchange mechanism of arsenic with nitrogen atoms at the GaN/GaAs interface and the phenomenon of quasi-saturation of the process observed experimentally.

Effect of oxygen plasma on nanomechanical silicon nitride resonators

NASA Astrophysics Data System (ADS)

Luhmann, Niklas; Jachimowicz, Artur; Schalko, Johannes; Sadeghi, Pedram; Sauer, Markus; Foelske-Schmitz, Annette; Schmid, Silvan

2017-08-01

Precise control of tensile stress and intrinsic damping is crucial for the optimal design of nanomechanical systems for sensor applications and quantum optomechanics in particular. In this letter, we study the influence of oxygen plasma on the tensile stress and intrinsic damping of nanomechanical silicon nitride resonators. Oxygen plasma treatments are common steps in micro and nanofabrication. We show that oxygen plasma for only a few minutes oxidizes the silicon nitride surface, creating several nanometer thick silicon dioxide layers with a compressive stress of 1.30(16) GPa. Such oxide layers can cause a reduction in the effective tensile stress of a 50 nm thick stoichiometric silicon nitride membrane by almost 50%. Additionally, intrinsic damping linearly increases with the silicon dioxide film thickness. An oxide layer of 1.5 nm grown in just 10 s in a 50 W oxygen plasma almost doubled the intrinsic damping. The oxide surface layer can be efficiently removed in buffered hydrofluoric acid.

Growth kinetics for temperature-controlled atomic layer deposition of GaN using trimethylgallium and remote-plasma-excited NH3

NASA Astrophysics Data System (ADS)

Pansila, P.; Kanomata, K.; Miura, M.; Ahmmad, B.; Kubota, S.; Hirose, F.

2015-12-01

Fundamental surface reactions in the atomic layer deposition of GaN with trimethylgallium (TMG) and plasma-excited NH3 are investigated by multiple-internal-reflection infrared absorption spectroscopy (MIR-IRAS) at surface temperatures varying from room temperature (RT) to 400 °C. It is found that TMG is saturated at RT on GaN surfaces when the TMG exposure exceeds 8 × 104 Langmuir (L), where 1 L corresponds to 1.33 × 10-4 Pa s (or 1.0 × 10-6 Torr s), and its saturation density reaches the maximum value at RT. Nitridation with the plasma-excited NH3 on the TMG-saturated GaN surface is investigated by X-ray photoelectron spectroscopy (XPS). The nitridation becomes effective at surface temperatures in excess of 100 °C. The reaction models of TMG adsorption and nitridation on the GaN surface are proposed in this paper. Based on the surface analysis, a temperature-controlled ALD process consisting of RT-TMG adsorption and nitridation at 115 °C is examined, where the growth per cycle of 0.045 nm/cycle is confirmed. XPS analysis indicates that all N atoms are bonded as GaN. Atomic force microscopy indicates an average roughness of 0.23 nm. We discuss the reaction mechanism of GaN ALD in the low-temperature region at around 115 °C with TMG and plasma-excited NH3.

Silicon solar cells made by a self-aligned, selective-emitter, plasma-etchback process

DOEpatents

Ruby, Douglas S.; Schubert, William K.; Gee, James M.

1999-01-01

A potentially low-cost process for forming and passivating a selective emitter. The process uses a plasma etch of the heavily doped emitter to improve its performance. The grids of the solar cell are used to mask the plasma etch so that only the emitter in the region between the grids is etched, while the region beneath the grids remains heavily doped for low contact resistance. This process is potentially low-cost because it requires no alignment. After the emitter etch, a silicon nitride layer is deposited by plasma-enhanced, chemical vapor deposition, and the solar cell is annealed in a forming gas.

Silicon solar cells made by a self-aligned, selective-emitter, plasma-etchback process

DOEpatents

Ruby, D.S.; Schubert, W.K.; Gee, J.M.

1999-02-16

A potentially low-cost process for forming and passivating a selective emitter. The process uses a plasma etch of the heavily doped emitter to improve its performance. The grids of the solar cell are used to mask the plasma etch so that only the emitter in the region between the grids is etched, while the region beneath the grids remains heavily doped for low contact resistance. This process is potentially low-cost because it requires no alignment. After the emitter etch, a silicon nitride layer is deposited by plasma-enhanced, chemical vapor deposition, and the solar cell is annealed in a forming gas. 5 figs.

Trap density of GeNx/Ge interface fabricated by electron-cyclotron-resonance plasma nitridation

NASA Astrophysics Data System (ADS)

Fukuda, Yukio; Otani, Yohei; Toyota, Hiroshi; Ono, Toshiro

2011-07-01

We have investigated GeNx/Ge interface properties using Si3N4(7 nm)/GeNx(2 nm)/Ge metal-insulator-semiconductor structures fabricated by the plasma nitridation of Ge substrates using an electron-cyclotron-resonance-generated nitrogen plasma. The interface trap density (Dit) measured by the conductance method is found to be distributed symmetrically in the Ge band gap with a minimum Dit value lower than 3 × 1011 cm-2eV-1 near the midgap. This result may lead to the development of processes for the fabrication of p- and n-Ge Schottky-barrier (SB) source/drain metal-insulator-semiconductor field-effect transistors using chemically and thermally robust GeNx dielectrics as interlayers for SB source/drain contacts and high-κ gate dielectrics.

Combined surface hardening and laser patterning approach for functionalising stainless steel surfaces

NASA Astrophysics Data System (ADS)

Garcia-Giron, A.; Romano, J. M.; Liang, Y.; Dashtbozorg, B.; Dong, H.; Penchev, P.; Dimov, S. S.

2018-05-01

The paper reports a laser patterning method for producing surfaces with dual scale topographies on ferritic stainless steel plates that are hardened by low temperature plasma surface alloying. Nitrogen and carbon based gasses were used in the alloying process to obtain surface layers with an increased hardness from 172 HV to 1001 HV and 305 HV, respectively. Then, a nanosecond infrared laser was used to pattern the plasma treated surfaces and thus to obtain super-hydrophobicity, by creating cell- or channel-like surface structures. The combined surface hardening and laser patterning approach allowed super-hydrophobic surfaces to be produced on both nitrided and carburised stainless steel plates with effective contact angles higher than 150°. The hardened layers on nitrided samples had cracks and was delaminated after the laser patterning while on plasma carburised samples remained intact. The results showed that by applying the proposed combined approach it is possible to retain the higher hardness of the nitrided stainless steel plates and at the same time to functionalise them to obtain super-hydrophobic properties.

Formation of Equiaxed Alpha and Titanium Nitride Precipitates in Spark Plasma Sintered TiB/Ti-6Al-4V Composites (Preprint)

DTIC Science & Technology

2012-08-01

AFRL-RX-WP-TP-2012-0372 FORMATION OF EQUIAXED ALPHA AND TITANIUM NITRIDE PRECIPITATES IN SPARK PLASMA SINTERED TiB/Ti-6Al-4V COMPOSITES...ALPHA AND TITANIUM NITRIDE PRECIPITATES IN SPARK PLASMA SINTERED TiB/Ti-6Al-4V COMPOSITES (PREPRINT) 5a. CONTRACT NUMBER FA8650-08-C-5226 5b...distribution of TiN precipitates, as revealed by TEM studies. 15. SUBJECT TERMS Ti-6Al-4V; TiB; TiN; Spark Plasma Sintering ; Composite; α/β phase

Corrosion Behavior of Active Screen Plasma Nitrided 38CrMoAl Steel under Marine Environment

NASA Astrophysics Data System (ADS)

Yang, Li; He, Yongyong; Mao, JunYuan; Zhang, Lei

2017-10-01

The 38CrMoAl steels were nitrided at different temperatures for 7 h using active screen plasma discharge. The analysis showed that the thick compound layer composed of ɛ-Fe2-3N and γ‧-Fe4N was formed on the surface. The corrosion behavior was evaluated by measuring the anodic polarization curves in natural sea water (similar 3.5% NaCl solution), and observation of corroded surface were conducted. The electromechanical measurements indicated that the corrosion potential of the nitrided specimens shifted to a nobler value compared to that of untreated specimens. Passive regions were also observed in the polarization curves for all the nitrided specimens. These results indicate that active screen plasma nitriding can enhance the corrosion resistance of the 38CrMoAl steel under marine environment.

Selective emitter solar cell formation by NH3 plasma nitridation and single diffusion

NASA Astrophysics Data System (ADS)

Wu, Yung-Hsien; Chen, Lun-Lun; Wu, Jia-Rong; Wu, Min-Lin

2010-01-01

A new and simple process for fabricating a selective emitter solar cell has been proposed. Lightly and heavily doped emitters could be concurrently formed after a single POCl3 diffusion step through the selective formation of SiNx, which serves as the diffusion barrier and can be grown by NH3 plasma nitridation of the Si surface. The desired phosphorus depth profile for the lightly and heavily doped region verifies the eligibility of this process. From the electrical characterization, the selective emitter solar cell fabricated by this process manifests a higher absolute conversion efficiency than a conventional one by 0.5%. It is the enhanced response to the short wavelength light and the reduced surface recombination that causes the considerable improvement in conversion efficiency which is beneficial to further hold the competitive advantage for solar cell manufacturers. Most importantly, the proposed process can be fully integrated into the conventional solar cell process in a mass-production laboratory.

Manufacturing of composite titanium-titanium nitride coatings by reactive very low pressure plasma spraying (R-VLPPS)

NASA Astrophysics Data System (ADS)

Vautherin, B.; Planche, M.-P.; Quet, A.; Bianchi, L.; Montavon, G.

2014-11-01

Very Low Pressure Plasma Spraying (VLPPS) is an emerging spray process nowadays intensively studied by many research centers in the World. To date, studies are mostly focused on the manufacturing of ceramic or metallic coatings. None refers to composite coatings manufacturing by reactive plasma spraying under very low pressure (i.e., ~150 Pa). This paper aims at presenting the carried-out developments and some results concerning the manufacturing of composite coatings by reactive spraying. Titanium was selected as metallic material in order to deposit titanium-nitride titanium coatings (Ti-TiN). Nitrogen was used as plasma gas and was injected along an Ar-H2-N2 plasma jet via a secondary injector in order to reach the nitrogen content on the substrate surface. Thus, different kind of reactive mechanisms were highlighted. Resulting coatings were characterized by Scanning Electron Microscopy (SEM) observations. Porous microstructures are clearly identified and the deposits exhibit condensed vapours and molten particles. Glow Discharge Optical Emission Spectroscopy (GDOES) analysis evidenced nitrogen inside the deposits and X-Ray Diffraction (XRD) analysis confirmed the formation of titanium nitride phases, such as TiN and Ti2N, depending upon the location of the nitrogen injection. Microhardness values as high as 800 VHN were measured on manufactured samples (to be compared to 220 VHN for pure titanium VLPPS-manufactured coatings).

Friction and Wear of Unlubricated NiTiHf with Nitriding Surface Treatments

NASA Technical Reports Server (NTRS)

Stanford, Malcolm K.

2018-01-01

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.

Modification of Low-Alloy Steel Surface by High-Temperature Gas Nitriding Plus Tempering

NASA Astrophysics Data System (ADS)

Jiao, Dongling; Li, Minsong; Ding, Hongzhen; Qiu, Wanqi; Luo, Chengping

2018-02-01

The low-alloy steel was nitrided in a pure NH3 gas atmosphere at 640 660 °C for 2 h, i.e., high-temperature gas nitriding (HTGN), followed by tempering at 225 °C, which can produce a high property surface coating without brittle compound (white) layer. The steel was also plasma nitriding for comparison. The composition, microstructure and microhardness of the nitrided and tempered specimens were examined, and their tribological behavior investigated. The results showed that the as-gas-nitrided layer consisted of a white layer composed of FeN0.095 phase (nitrided austenite) and a diffusional zone underneath the white layer. After tempering, the white layer was decomposed to a nano-sized (α-Fe + γ'-Fe4N + retained austenite) bainitic microstructure with a high hardness of 1150HV/25 g. Wear test results showed that the wear resistance and wear coefficient yielded by the complex HTGN plus tempering were considerably higher and lower, respectively, than those produced by the conventional plasma nitriding.

Method and device to synthesize boron nitride nanotubes and related nanoparticles

DOEpatents

Zettl, Alexander K.

2016-07-19

Methods and apparatus for producing chemical nanostructures having multiple elements, such as boron and nitride, e.g. boron nitride nanotubes, are disclosed. The method comprises creating a plasma jet, or plume, such as by an arc discharge. The plasma plume is elongated and has a temperature gradient along its length. It extends along its length into a port connector area having ports for introduction of feed materials. The feed materials include the multiple elements, which are introduced separately as fluids or powders at multiple ports along the length of the plasma plume, said ports entering the plasma plume at different temperatures. The method further comprises modifying a temperature at a distal portion of or immediately downstream of said plasma plume; and collecting said chemical nanostructures after said modifying.

Dynamic determination of secondary electron emission using a calorimetric probe in a plasma immersion ion implantation experiment

NASA Astrophysics Data System (ADS)

Haase, Fabian; Manova, Darina; Hirsch, Dietmar; Mändl, Stephan; Kersten, Holger

2018-04-01

A passive thermal probe has been used to detect dynamic changes in the secondary electron emission (SEE). Oxidized and nitrided materials have been studied during argon ion sputtering in a plasma immersion ion implantation process. Identical measurements have been performed for the metallic state with high voltage pulses accelerating nitrogen ions towards the surface, supposedly forming a nitride layer. Energy flux data were combined with scanning electron microscopy images of the surface to obtain information about the actual surface composition as well as trends and changes during the process. Within the measurements, a direct comparison of the SEE within both employed ion species (argon and nitrogen) is possible while an absolute quantification is still open. Additionally, the nominal composition of the investigated oxide and nitride layers does not always correspond to stoichiometric compounds. Nevertheless, the oxides showed a remarkably higher SEE compared to the pure metals, while an indistinct behavior was observed for the nitrides: some higher, some lower than the clean metal surfaces. For the aluminum alloy AlMg3 a complex time dependent evolution was observed with consecutive oxidation/sputtering cycles leading to a very rough surface with a diminished oxide layer, leading to an almost black surface of the metal and non-reproducible changes in the SEE. The presented method is a versatile technique for measuring dynamic changes of the surface for materials commonly used in PVD processes with a time resolution of about 1 min, e.g. magnetron sputtering or HiPIMS, where changes in the target or electrode composition are occurring but cannot be measured directly.

Fully CMOS-compatible titanium nitride nanoantennas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Briggs, Justin A., E-mail: jabriggs@stanford.edu; Department of Materials Science and Engineering, Stanford University, 496 Lomita Mall, Stanford, California 94305; Naik, Gururaj V.

CMOS-compatible fabrication of plasmonic materials and devices will accelerate the development of integrated nanophotonics for information processing applications. Using low-temperature plasma-enhanced atomic layer deposition (PEALD), we develop a recipe for fully CMOS-compatible titanium nitride (TiN) that is plasmonic in the visible and near infrared. Films are grown on silicon, silicon dioxide, and epitaxially on magnesium oxide substrates. By optimizing the plasma exposure per growth cycle during PEALD, carbon and oxygen contamination are reduced, lowering undesirable loss. We use electron beam lithography to pattern TiN nanopillars with varying diameters on silicon in large-area arrays. In the first reported single-particle measurements onmore » plasmonic TiN, we demonstrate size-tunable darkfield scattering spectroscopy in the visible and near infrared regimes. The optical properties of this CMOS-compatible material, combined with its high melting temperature and mechanical durability, comprise a step towards fully CMOS-integrated nanophotonic information processing.« less

Optimization of process parameters in the RF-DC plasma N2-H2 for AISI420 molds and dies

NASA Astrophysics Data System (ADS)

Herdianto, Hengky; Djoko, D. J.; Santjojo, H.; Masruroh

2017-11-01

The RF-DC plasma N2-H2 was used to make precise AISI420 molds and dies have complex textured geometry. The quality of the molds and dies directly affect the quality of the produced parts. The excellent examples of molds were used for injection molding lenses and dies used for the precision forging of automotive drive train components. In this study, a temperature, DC bias, and duration as process parameters of the RF-DC plasma N2-H2 have been optimized for molds and dies fabrication. The mask-less micro-patterned method was utilized to draw the initial 2D micro patterns directly onto the AISI420 substrate surface. The unprinted substrate surfaces were selectively nitrided by the RF-DC plasma N2-H2 at 673 K for 5400 s by 70 Pa with hollow cathode device. Energy Dispersive X-ray was utilized to describe the nitrogen content distribution at the vicinity of the border between the unprinted surfaces. This exclusive nitrogen mapping proves that only the unprinted parts of the substrate have high content nitrogen solutes. XRD analysis was performed to investigate whether the iron nitrides were precipitated by RF-DC plasma N2-H2 in the AISI420.

Nitrogen Plasma Optimization for High-Quality Dilute Nitrides

DTIC Science & Technology

2005-02-01

Available online 1 February 2005Abstract Growth of GaInNAs by molecular beam epitaxy (MBE) generally requires a nitrogen plasma, which complicates growth...InGaAs and InGaAsP lasers. This paper addresses several of the challenges of plasma-assisted molecular beam epitaxy (MBE) of high-quality dilute nitrides...A.L. Holmes, Using beam flux monitor as Langmuir probe for plasma-assisted molecular beam epitaxy , J. Vac. Sci. Technol. B, in press.

Alternative process for thin layer etching: Application to nitride spacer etching stopping on silicon germanium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Posseme, N., E-mail: nicolas.posseme@cea.fr; Pollet, O.; Barnola, S.

2014-08-04

Silicon nitride spacer etching realization is considered today as one of the most challenging of the etch process for the new devices realization. For this step, the atomic etch precision to stop on silicon or silicon germanium with a perfect anisotropy (no foot formation) is required. The situation is that none of the current plasma technologies can meet all these requirements. To overcome these issues and meet the highly complex requirements imposed by device fabrication processes, we recently proposed an alternative etching process to the current plasma etch chemistries. This process is based on thin film modification by light ionsmore » implantation followed by a selective removal of the modified layer with respect to the non-modified material. In this Letter, we demonstrate the benefit of this alternative etch method in term of film damage control (silicon germanium recess obtained is less than 6 A), anisotropy (no foot formation), and its compatibility with other integration steps like epitaxial. The etch mechanisms of this approach are also addressed.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Souza, S.D. de; Olzon-Dionysio, M., E-mail: dmod@df.ufscar.br; Basso, R.L.O.

2010-10-15

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 broadmore » {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.« less

Fabrication of Ta2O5/GeNx gate insulator stack for Ge metal-insulator-semiconductor structures by electron-cyclotron-resonance plasma nitridation and sputtering deposition techniques

NASA Astrophysics Data System (ADS)

Otani, Yohei; Itayama, Yasuhiro; Tanaka, Takuo; Fukuda, Yukio; Toyota, Hiroshi; Ono, Toshiro; Mitsui, Minoru; Nakagawa, Kiyokazu

2007-04-01

The authors have fabricated germanium (Ge) metal-insulator-semiconductor (MIS) structures with a 7-nm-thick tantalum pentaoxide (Ta2O5)/2-nm-thick germanium nitride (GeNx) gate insulator stack by electron-cyclotron-resonance plasma nitridation and sputtering deposition. They found that pure GeNx ultrathin layers can be formed by the direct plasma nitridation of the Ge surface without substrate heating. X-ray photoelectron spectroscopy revealed no oxidation of the GeNx layer after the Ta2O5 sputtering deposition. The fabricated MIS capacitor with a capacitance equivalent thickness of 4.3nm showed excellent leakage current characteristics. The interface trap density obtained by the modified conductance method was 4×1011cm-2eV-1 at the midgap.

Effect of pulsed duty cycle control on tribological and corrosion properties of AISI-316 in cathodic cage plasma nitriding

NASA Astrophysics Data System (ADS)

Naeem, M.; Raza, H. A.; Shafiq, M.; Zaka-ul-Islam, M.; Iqbal, Javed; Díaz-Guillén, J. C.; Zakaullah, M.

2017-11-01

Austenitic stainless steels are of prime importance in many industrial sectors because of their excellent corrosion resistance; however, their poor mechanical and tribological features lead to their reduced applicability. In this regard, low-temperature cathodic cage plasma nitriding (CCPN) can be used to improve surface properties of steels without scarifying the inherent corrosion resistance. In this study, AISI-316 samples are processed in CCPN reactor at a temperature of 400 °C, for the treatment time of 4 h, at a pressure of 150 Pa and variable pulsed duty cycle (15-75%). The microstructure and mechanical features are analyzed using x-ray diffraction, scanning electron microscopy, microhardness tester and ball-on-disc wear tester. The anodic polarization test in 3.5% NaCl is conducted to examine the corrosion properties. The results show that hardness is enhanced up to 1327 HV at low duty cycle, which is considerably higher than base material (278 HV). The wear rate is found to be reduced up to 90% over base material by processing at low duty cycle. The base material exhibits severe abrasive wear, and the nitrided sample has dominant adhesive wear. The corrosion rate is found to be reduced up to 95% over base material for the sample nitrided at low duty cycle. This study shows that wear and corrosion resistance in CCPN can be significantly boosted by reducing the pulsed duty cycle.

Enhanced cell adhesion on severe peened-plasma nitrided 316L stainless steel

NASA Astrophysics Data System (ADS)

Jayalakshmi, M.; Bhat, Badekai Ramachandra; Bhat, K. Udaya

2018-04-01

Plasma nitriding is an effective technique to enhance the wear resistance of austenitic stainless steels. Recently, severe surface deformation techniques are extensively used prior to nitriding to enhance diffusion kinetics. In the present study, AISI 316L austenitic stainless steel is subjected to peening-nitriding duplex treatment and biocompatibility of treated surfaces is assessed through adhesion of the fibroblast cells. Three-fold increase in the surface microhardness is observed from the un-peened sample to the peened-nitrided sample; with severe peened sample showing intermediate hardness. Similar trend is observed in the number of the fibroblast cells attached to the sample surface. Spreading of some of the fibroblast cells is observed on the sample subjected to duplex treatment; while the other two samples showed only the spindle shaped fibroblasts. Combined influence of surface nanocrystallization and presence of nitride layer is responsible for the improved biocompatibility.

Conversion electron Mössbauer spectroscopy of plasma immersion ion implanted H13 tool steel

NASA Astrophysics Data System (ADS)

Terwagne, G.; Collins, G. A.; Hutchings, R.

1994-12-01

Conversion electron Mössbauer spectroscopy (CEMS) has been used to investigate nitride formation in AISI-H13 tool steel after treatment by plasma immersion ion implantation (PI3) at 350 °C. With only slight variation in the plasma conditions, it is possible to influence the kinetics of nitride precipitation so as to obtain nitrogen concentrations that range from those associated with ɛ-Fe2N through ɛ-Fe3N to γ'-Fe4N. The CEMS results enable a more definite identification of the nitrides than that obtained by glancing-angle X-ray diffraction and nuclear reaction analysis alone.

Deuterated silicon nitride photonic devices for broadband optical frequency comb generation

NASA Astrophysics Data System (ADS)

Chiles, Jeff; Nader, Nima; Hickstein, Daniel D.; Yu, Su Peng; Briles, Travis Crain; Carlson, David; Jung, Hojoong; Shainline, Jeffrey M.; Diddams, Scott; Papp, Scott B.; Nam, Sae Woo; Mirin, Richard P.

2018-04-01

We report and characterize low-temperature, plasma-deposited deuterated silicon nitride thin films for nonlinear integrated photonics. With a peak processing temperature less than 300$^\\circ$C, it is back-end compatible with pre-processed CMOS substrates. We achieve microresonators with a quality factor of up to $1.6\\times 10^6 $ at 1552 nm, and $>1.2\\times 10^6$ throughout $\\lambda$ = 1510 -- 1600 nm, without annealing or stress management. We then demonstrate the immediate utility of this platform in nonlinear photonics by generating a 1 THz free spectral range, 900-nm-bandwidth modulation-instability microresonator Kerr comb and octave-spanning, supercontinuum-broadened spectra.

Process parameter-growth environment-film property relationships for reactive sputter deposited metal (V, Nb, Zr, Y, Au) oxide, nitride, and oxynitride films. Final report, 1 January 1989-30 June 1993

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aita, C.R.

1993-09-30

The research developed process parameter-growth environment-film property relations (phase maps) for model sputter-deposited transition metal oxides, nitrides, and oxynitrides grown by reactive sputter deposition at low temperature. Optical emission spectrometry was used for plasma diagnostics. The results summarized here include the role of sputtered metal-oxygen molecular flux in oxide film growth; structural differences in highest valence oxides including conditions for amorphous growth; and using fundamental optical absorption edge features to probe short range structural disorder. Eight appendices containing sixteen journal articles are included.

Simple realization of efficient barrier performance of a single layer silicon nitride film via plasma chemistry.

PubMed

Lee, Jun Suk; Sahu, Bibhuti Bhusan; Han, Jeon Geon

2016-11-30

Due to the problem of degradation by moisture or oxygen, there is growing interest in efficient gas diffusion barriers for organic optoelectronic devices. Additionally, for the continuous and long-term operation of a device, dedicated flexible thin film encapsulation is required, which is the foremost challenge. Many efforts are being undertaken in the plasma assisted deposition process control for the optimization of film properties. Control of the plasma density along with the energy of the principal plasma species is critical to inducing alteration of the plasma reactivity, chemistry, and film properties. Here, we have used the radio frequency (RF) plasma enhanced chemical vapor deposition (PECVD) technique to deposit amorphous silicon nitride (SiN x ) barrier films onto a plastic substrate at different pressures. A large part of our efforts is devoted to a detailed study of the process parameters controlling the plasma treatment. Numerous plasma diagnostic techniques combined with various characterization tools are purposefully used to characterize and investigate the plasma environment and the associated film properties. This contribution also reports a study of the correlations between the plasma chemistry and the chemical, mechanical, barrier, and optical properties of the deposited films. The data reveal that the film possesses a very low stress for the condition where the net energy imparted on the substrate is at a minimum. Simultaneously, a relatively high ion flux and high energy of the ions impinging on the film growth surfaces are crucial for controlling the film stress and the resulting barrier properties.

Taguchi Analysis on the Effect of Process Parameters on Densification During Spark Plasma Sintering of HfB2-20SiC (Preprint)

DTIC Science & Technology

2011-11-01

30 kN pressure and heating rate of 100 K/min. Introduction Boride , carbides and nitrides of the group IVB and VB transition metals are considered...10. Sciti D., Silvestroni L., Nygren M. Spark plasma sintering of Zr- and Hf- borides with decreasing amounts of MoSi2 as sintering aid Journal of

Method for forming ammonia

DOEpatents

Kong, Peter C.; Pink, Robert J.; Zuck, Larry D.

2008-08-19

A method for forming ammonia is disclosed and which includes the steps of forming a plasma; providing a source of metal particles, and supplying the metal particles to the plasma to form metal nitride particles; and providing a substance, and reacting the metal nitride particles with the substance to produce ammonia, and an oxide byproduct.

Radio Frequency Plasma Synthesis of Boron Nitride Nanotubes (BNNTs) for Structural Applications: Part I

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Alexa, Joel A.; Jensen, Brian J.; Thomsen, Donald L.

2016-01-01

It is evident that nanotubes, such as carbon, boron nitride and even silicon, offer great potential for many aerospace applications. The opportunity exists to harness the extremely high strength and stiffness exhibited by high-purity, low-defect nanotubes in structural materials. Even though the technology associated with carbon nanotube (CNT) development is mature, the mechanical property benefits have yet to be fully realized. Boron nitride nanotubes (BNNTs) offer similar structural benefits, but exhibit superior chemical and thermal stability. A broader range of potential structural applications results, particularly as reinforcing agents for metal- and ceramic- based composites. However, synthesis of BNNTs is more challenging than CNTs mainly because of the higher processing temperatures required, and mass production techniques have yet to emerge. A promising technique is radio frequency plasma spray (RFPS), which is an inductively coupled, very high temperature process. The lack of electrodes and the self- contained, inert gas environment lend themselves to an ultraclean product. It is the aim of this White Paper to survey the state of the art with regard to nano-material production by analyzing the pros and cons of existing methods. The intention is to combine the best concepts and apply the NASA Langley Research Center (LaRC) RFPS facility to reliably synthesize large quantities of consistent, high-purity BNNTs.

The Influence of Plasma-Based Nitriding and Oxidizing Treatments on the Mechanical and Corrosion Properties of CoCrMo Biomedical Alloy

NASA Astrophysics Data System (ADS)

Noli, Fotini; Pichon, Luc; Öztürk, Orhan

2018-04-01

Plasma-based nitriding and/or oxidizing treatments were applied to CoCrMo alloy to improve its surface mechanical properties and corrosion resistance for biomedical applications. Three treatments were performed. A set of CoCrMo samples has been subjected to nitriding at moderate temperatures ( 400 °C). A second set of CoCrMo samples was oxidized at 395 °C in pure O2. The last set of CoCrMo samples was nitrided and subsequently oxidized under the experimental conditions of previous sets (double treatment). The microstructure and morphology of the layers formed on the CoCrMo alloy were investigated by X-ray diffraction, Atomic Force Microscopy, and Scanning Electron Microscopy. In addition, nitrogen and oxygen profiles were determined by Glow Discharge Optical Emission Spectroscopy, Rutherford Backscattering Spectroscopy, Energy-Dispersive X-ray, and Nuclear Reaction Analysis. Significant improvement of the Vickers hardness of the CoCrMo samples after plasma nitriding was observed due to the supersaturated nitrogen solution and the formation of an expanded FCC γ N phase and CrN precipitates. In the case of the oxidized samples, Vickers hardness improvement was minimal. The corrosion behavior of the samples was investigated in simulated body fluid (0.9 pct NaCl solution at 37 °C) using electrochemical techniques (potentiodynamic polarization and cyclic voltammetry). The concentration of metal ions released from the CoCrMo surfaces was determined by Instrumental Neutron Activation Analysis. The experimental results clearly indicate that the CoCrMo surface subjected to the double surface treatment consisting in plasma nitriding and plasma oxidizing exhibited lower deterioration and better resistance to corrosion compared to the nitrided, oxidized, and untreated samples. This enhancement is believed to be due to the formation of a thicker and more stable layer.

Pseudo-Capacitors: SPPS Deposition and Electrochemical Analysis of α-MoO3 and Mo2N Coatings

NASA Astrophysics Data System (ADS)

Golozar, Mehdi; Chien, Ken; Lian, Keryn; Coyle, Thomas W.

2013-06-01

Solution precursor plasma spraying (SPPS) is a novel thermal spray process in which a solution precursor is injected into the high-temperature zone of a DC-arc plasma jet to allow solvent evaporation from the precursor droplets, solute precipitation, and precipitate pyrolysis prior to substrate impact. This investigation explored the potential of SPPS to fabricate α-MoO3 coatings with fine grain sizes, high porosity levels, and high surface area: characteristics needed for application as pseudo-capacitor electrodes. Since molybdenum nitride has shown a larger electrochemical stability window and higher specific area capacitance, the α-MoO3 deposits were subsequently converted into molybdenum nitride. A multistep heat-treatment procedure resulted in a topotactic phase-transformation mechanism, which retained the high surface area lath-shaped features of the original α-MoO3. The electrochemical behaviors of molybdenum oxide and molybdenum nitride deposits formed under different deposition conditions were studied using cyclic voltammetry to assess the influence of the resulting microstructure on the charge storage behavior and potential for use in pseudo-capacitors.

Extraction of titanium from low-iron nitrided Malaysian ilmenite by chlorination

NASA Astrophysics Data System (ADS)

Ibrahim, Najwa; Ahmadi, Eltefat; Rahman, Shaik Abdul; Fauzi, M. N. Ahmad; Rezan, Sheikh Abdul

2017-01-01

In this paper, production of TiCl4 from low-iron nitrided ilmenite samples at relatively low temperature using chlorine gas generated from the reaction between KMnO4 and HCl has been investigated. The effects of chlorination soaking time, potassium permanganate (KMnO4) to hydrochloric acid (HCl) molar ratio and aluminium powder catalyst in chlorine gas generation on titanium extraction from nitrided Malaysian ilmenite were examined. The low-iron nitrided Malaysian ilmenite contained titanium oxycarbonitride (TiOxCyNz) after carbothermal reduction and nitridation with subsequent leaching. Chlorination process was performed at 500°C for 30 - 60 minutes. Statistical analysis of the data was done by Design of Experiment (DOE) to identify the significant variables and their interactions. The results achieved in this study showed that the highest extent of chlorination was about 98.34% at 500°C for 60 minutes. The lowest extent of chlorination was about 68.51% obtained in KMnO4 to HCl molar ratio of 2.0 and 0.35 g of aluminium powder. The chlorinated titanium oxycarbonitride powders and TiCl4 solutions were analyzed by X-ray diffraction (XRD) and inductively coupled plasma-optical emission spectroscopy (ICP-OES), respectively. The purpose of this study was to explore the relationship between the processing parameters on extracting titanium via pyrometallurgical technique.

Early stages of plasma induced nitridation of Si (111) surface and study of interfacial band alignment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shetty, Satish; Shivaprasad, S. M., E-mail: smsprasad@jncasr.ac.in

2016-02-07

We report here a systematic study of the nitridation of the Si (111) surface by nitrogen plasma exposure. The surface and interface chemical composition and surface morphology are investigated by using RHEED, X-ray photoelectron spectroscopy, and atomic force microscopy (AFM). At the initial stage of nitridation two superstructures—“8 × 8” and “8/3 × 8/3”—form, and further nitridation leads to 1 × 1 stoichiometric silicon nitride. The interface is seen to have the Si{sup 1+} and Si{sup 3+} states of silicon bonding with nitrogen, which suggests an atomically abrupt and defect-free interface. The initial single crystalline silicon nitride layers are seen to become amorphous at higher thicknesses.more » The AFM image shows that the nitride nucleates at interfacial dislocations that are connected by sub-stoichiometric 2D-nitride layers, which agglomerate to form thick overlayers. The electrical properties of the interface yield a valence band offset that saturates at 1.9 eV and conduction band offset at 2.3 eV due to the evolution of the sub-stoichiometric interface and band bending.« less

Surface Modification of C17200 Copper-Beryllium Alloy by Plasma Nitriding of Cu-Ti Gradient Film

NASA Astrophysics Data System (ADS)

Zhu, Y. D.; Yan, M. F.; Zhang, Y. X.; Zhang, C. S.

2018-03-01

In the present work, a copper-titanium film of gradient composition was firstly fabricated by the dual magnetron sputtering through power control and plasma nitriding of the film was then conducted to modify C17200 Cu alloy. The results showed that the prepared gradient Cu-Ti film by magnetron sputtering was amorphous. After plasma nitriding at 650 °C, crystalline Cu-Ti intermetallics appeared in the multi-phase coating, including CuTi2, Cu3Ti, Cu3Ti2 and CuTi. Moreover, even though the plasma nitriding duration of the gradient Cu-Ti film was only 0.5 h, the mechanical properties of the modified Cu surface were obviously improved, with the surface hardness enhanced to be 417 HV0.01, the wear rate to be 0.32 × 10-14 m3/Nm and the friction coefficient to be 0.075 at the load of 10 N, which are all more excellent than the C17200 Cu alloy. In addition, the wear mechanism also changed from adhesion wear for C17200 Cu substrate to abrasive wear for the modified surface.

Organometallic chemical vapor deposition of silicon nitride films enhanced by atomic nitrogen generated from surface-wave plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Okada, H.; Kato, M.; Ishimaru, T.

2014-02-20

Organometallic chemical vapor deposition of silicon nitride films enhanced by atomic nitrogen generated from surface-wave plasma is investigated. Feasibility of precursors of triethylsilane (TES) and bis(dimethylamino)dimethylsilane (BDMADMS) is discussed based on a calculation of bond energies by computer simulation. Refractive indices of 1.81 and 1.71 are obtained for deposited films with TES and BDMADMS, respectively. X-ray photoelectron spectroscopy (XPS) analysis of the deposited film revealed that TES-based film coincides with the stoichiometric thermal silicon nitride.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Borkar, Tushar; Nag, Soumya; Ren, Yang

Coupled in situ alloying and nitridation of titanium–vanadium alloys, has been achieved by introducing reactive nitrogen gas during the spark plasma sintering (SPS) of blended titanium and vanadium elemental powders, leading to a new class of nitride reinforced titanium alloy composites. The resulting microstructure includes precipitates of the d-TiN phase with the NaCl structure, equiaxed (or globular) precipitates of a nitrogen enriched hcp a(Ti,N) phase with a c/a ratio more than what is expected for pure hcp Ti, and fine scale plate-shaped precipitates of hcp a-Ti, distributed within a bcc b matrix. During SPS processing, the d-TiN phase appears tomore » form at a temperature of 1400 C, while only hcp a(Ti,N) and a-Ti phases form at lower processing temperatures. Consequently, the highest microhardness is exhibited by the composite processed at 1400 C while those processed at 1300 C or below exhibit lower values. Processing at temperatures below 1300 C, resulted in an incomplete alloying of the blend of titanium and vanadium powders. These d-TiN precipitates act as heterogeneous nucleation sites for the a(Ti,N) precipitates that appear to engulf and exhibit an orientation relationship with the nitride phase at the center. Furthermore, fine scale a-Ti plates are precipitated within the nitride precipitates, presumably resulting from the retrograde solubility of nitrogen in titanium.« less

Formation of Wear Resistant Steel Surfaces by Plasma Immersion Ion Implantation

NASA Astrophysics Data System (ADS)

Mändl, S.; Rauschenbach, B.

2003-08-01

Plasma immersion ion implantation (PIII) is a versatile and fast method for implanting energetic ions into large and complex shaped three-dimensional objects where the ions are accelerated by applying negative high voltage pulses to a substrate immersed in a plasma. As the line-of-sight restrictions of conventional implanters are circumvented, it results in a fast and cost-effective technology. Implantation of nitrogen at 30 - 40 keV at moderate temperatures of 200 - 400 °C into steel circumvents the diminishing thermal nitrogen activation encountered, e.g., in plasma nitriding in this temperature regime, thus enabling nitriding of additional steel grades. Nitride formation and improvement of the mechanical properties after PIII are presented for several steel grades, including AISI 316Ti (food industry), AISI D2 (used for bending tools) and AISI 1095 (with applications in the textile industry).

Suppression of carbon desorption from 4H-SiC by irradiating a remote nitrogen plasma at a low temperature

NASA Astrophysics Data System (ADS)

Shimabayashi, Masaharu; Kurihara, Kazuaki; Sasaki, Koichi

2018-05-01

We remotely irradiated a nitrogen plasma onto the carbon-side surface of 4H-SiC at a low temperature, and examined the effect of sample cooling on the characteristics of the nitride layer. An improved nitride layer, which had higher concentrations of carbon and silicon and a lower concentration of oxygen, was formed in the region at depths of more than 0.6–0.9 nm from the top surface. The depth of the fragile nitride layer in the top region, where no improved characteristics of the nitride layer were observed, became smaller with sample cooling. In addition, on the basis of the experimental results, we discussed the difference in the activation energy of the nitriding reaction of 4H-SiC supported by atomic nitrogen and molecular nitrogen in the metastable \\text{A}3Σ \\text{u} + state.

Nitrogen-Doped Carbon Fiber Paper by Active Screen Plasma Nitriding and Its Microwave Heating Properties.

PubMed

Zhu, Naishu; Ma, Shining; Sun, Xiaofeng

2016-12-28

In this paper, active screen plasma nitriding (ASPN) treatment was performed on polyacrylonitrile carbon fiber papers. Electric resistivity and microwave loss factor of carbon fiber were described to establish the relationship between processing parameters and fiber's ability to absorb microwaves. The surface processing effect of carbon fiber could be characterized by dynamic thermal mechanical analyzer testing on composites made of carbon fiber. When the process temperature was at 175 °C, it was conducive to obtaining good performance of dynamical mechanical properties. The treatment provided a way to change microwave heating properties of carbon fiber paper by performing different treatment conditions, such as temperature and time parameters. Atomic force microscope, scanning electron microscope, and X-ray photoelectron spectroscopy analysis showed that, during the course of ASPN treatment on carbon fiber paper, nitrogen group was introduced and silicon group was removed. The treatment of nitrogen-doped carbon fiber paper represented an alternative promising candidate for microwave curing materials used in repairing and heating technology, furthermore, an efficient dielectric layer material for radar-absorbing structure composite in metamaterial technology.

Plasma induced sp 2 to sp 3 transition in boron nitride

NASA Astrophysics Data System (ADS)

Zhang, J.; Cui, Q.; Li, X.; He, Z.; Li, W.; Ma, Y.; Guan, Q.; Gao, W.; Zou, G.

2004-12-01

The transition from sp 2 to sp 3 hybridization in boron nitride has been induced in plasma. Nano-crystals of cubic boron nitride (cBN) have been synthesized by direct current arc discharge method using hexagonal boron nitride (hBN) as the starting material. The characterization of the as-grown powders is carried out by X-ray diffraction, Fourier transform infrared spectroscopy and transmission electron microscopy. It has been shown that cBN and hBN grains with 20-60 nm in size co-exist in the powders. A reaction route of sublimation - re-hybridization - crystallization had been put forward to explain the mechanism of the hybridization transition and the growth of cBN by this method.

Low temperature RF plasma nitriding of self-organized TiO2 nanotubes for effective bandgap reduction

NASA Astrophysics Data System (ADS)

Bonelli, Thiago Scremin; Pereyra, Inés

2018-06-01

Titanium dioxide is a widely studied semiconductor material found in many nanostructured forms, presenting very interesting properties for several applications, particularly photocatalysis. TiO2 nanotubes have a high surface-to-volume ratio and functional electronic properties for light harvesting. Despite these manifold advantages, TiO2 photocatalytic activity is limited to UV radiation due to its large band gap. In this work, TiO2 nanotubes produced by electrochemical anodization were submitted to plasma nitriding processes in a PECVD reactor. The plasma parameters were evaluated to find the best conditions for gap reduction, in order to increase their photocatalytic activity. The pressure and RF power density were varied from 0.66 to 2.66 mbar and 0.22 to 3.51 W/cm2 respectively. The best gap reduction, to 2.80 eV, was achieved using a pressure of 1.33 mbar and 1.75 W/cm2 RF power at 320 °C, during a 2-h process. This leads to a 14% reduction in the band gap value and an increase of 25.3% in methylene blue reduction, doubling the range of solar photons absorption from 5 to 10% of the solar spectrum.

Titanium-nitride-oxide-coated coronary stents: insights from the available evidence.

PubMed

Karjalainen, Pasi P; Nammas, Wail

2017-06-01

Coating of stent surface with a biocompatible material is suggested to improve stent safety profile. A proprietary process was developed to coat titanium-nitride-oxide on the stent surface, based on plasma technology that uses the nano-synthesis of gas and metal. Preclinical in vitro and in vivo investigation confirmed blood compatibility of titanium (nitride-) oxide films. Titanium-nitride-oxide-coated stents demonstrated a better angiographic outcome, compared with bare-metal stents at mid-term follow-up; however, they failed to achieve non-inferiority for angiographic outcome versus second-generation drug-eluting stents. Observational studies showed adequate clinical outcome at mid-term follow-up. Non-randomized studies showed an outcome of titanium-nitride-oxide-coated stents comparable to - or better than - first-generation drug-eluting stents at long-term follow-up. Two randomized controlled trials demonstrated comparable efficacy outcome, and a better safety outcome of titanium-nitride-oxide-coated stents versus drug-eluting stents at long-term follow-up. Evaluation by optical coherence tomography at mid-term follow-up revealed better neointimal strut coverage associated with titanium-nitride-oxide-coated stents versus drug-eluting stents; yet, neointimal hyperplasia thickness was greater. Key messages Stents coated with titanium-nitride-oxide demonstrated biocompatibility in preclinical studies: they inhibit platelet and fibrin deposition, and reduce neointimal growth. In observational and non-randomized studies, titanium-nitride-oxide-coated stents were associated with adequate safety and efficacy outcome. In randomized trials of patients with acute coronary syndrome, titanium-nitride-oxide-coated stents were associated with a better safety outcome, compared with drug-eluting stents; efficacy outcome was comparable.

Influence of interfaces density and thermal processes on mechanical stress of PECVD silicon nitride

NASA Astrophysics Data System (ADS)

Picciotto, A.; Bagolini, A.; Bellutti, P.; Boscardin, M.

2009-10-01

The paper focuses on a particular silicon nitride thin film (SiN x) produced by plasma enahanced chemical vapor deposition (PECVD) technique with high deposition rate (26 nm/min) and low values of mechanical stress (<100 MPa). This was perfomed with mixed frequency procedure varying the modulation of high frequency at 13.56 MHz and low frequency at 308 kHz of RF power supply during the deposition, without changing the ratio of reaction gases. Low stress silicon nitride is commonly obtained by tailoring the thickness ratio of high frequency vs. low frequency silicon nitride layers. The attention of this work was directed to the influence of the number of interfaces per thickness unit on the stress characteristics of the deposited material. Two sets of wafer samples were deposited with low stress silicon nitride, with a thickness of 260 nm and 2 μm, respectively. Thermal annealing processes at 380 and 520 °C in a inert enviroment were also performed on the wafers. The Stoney-Hoffman model was used to estimate the stress values by wafer curvature measurement with a mechanical surface profilometer: the stress was calculated for the as-deposited layer, and after each annealing process. The thickness and the refractive index of the SiN x were also measured and charaterized by variable angle spectra elliposometry (VASE) techinique. The experimental measurements were performed at the MT-LAB, IRST (Istituto per la Ricerca Scientifica e Tecnologica) of Bruno Kessler Foundation for Research in Trento.

Impact of In situ Postnitridation Annealing for Successful Fabrication of HfSiON Thin Film

NASA Astrophysics Data System (ADS)

Horii, Sadayoshi; Ishikawa, Dai; Sano, Atsushi; Imai, Yoshinori; Kunii, Yasuo

2007-05-01

For the successful integration of high-k gate dielectrics into advanced complementary metal-oxide-semiconductor (CMOS) processes, it is important to determine the stability of high-k materials during exposure to an ambient atmosphere. In this work, we investigated the effect of exposure to air on the nitrogen concentration in HfSiON films formed by sequentially combining HfSiO chemical vapor deposition (CVD), plasma nitridation, and postnitridation annealing (PNA). We observed that exposure to air after the nitridation step reduces the nitrogen concentration due to a reaction between the HfSiON surface and the constituents of atmospheric air. We also found that exposure to air for even a short time between nitridation and PNA leads to a significant loss of nitrogen concentration, indicating that in situ PNA is critical for achieving precise control of the nitridation. These results confirmed the importance of using clustered multichamber platforms for successful high-k fabrication.

Optical Boron Nitride Insulator Erosion Characterization of a 200 W Xenon Hall Thruster

DTIC Science & Technology

2005-05-01

Hall thruster boron nitride insulator is evaluated as a diagnostic for real-time evaluation of thruster insulator erosion. Three Hall thruster plasma control variables are examined: ion energy (discharge potential), ion flux (propellant flow), and plasma conductivity (magnetic field strength). The boron emission, and hence the insulator erosion rate, varies linearly with ion energy and ion flux. A minimum erosion rate appears at intermediate magnetic field strengths. This may indicate that local plasma conductivity significantly affects the divergence

Surface passivation of p-type Ge substrate with high-quality GeNx layer formed by electron-cyclotron-resonance plasma nitridation at low temperature

NASA Astrophysics Data System (ADS)

Fukuda, Yukio; Okamoto, Hiroshi; Iwasaki, Takuro; Otani, Yohei; Ono, Toshiro

2011-09-01

We have investigated the effects of the formation temperature and postmetallization annealing (PMA) on the interface properties of GeNx/p-Ge fabricated by the plasma nitridation of Ge substrates using an electron-cyclotron-resonance-generated nitrogen plasma. The nitridation temperature is found to be a critical parameter in improving the finally obtained GeNx/Ge interface properties. The GeNx/Ge formed at room temperature and treated by PMA at 400 °C exhibits the best interface properties with an interface trap density of 1 × 1011 cm-2 eV-1. The GeNx/Ge interface is unpinned and the Fermi level at the Ge surface can move from the valence band edge to the conduction band edge.

The role of plasma chemistry on functional silicon nitride film properties deposited at low-temperature by mixing two frequency powers using PECVD.

PubMed

Sahu, B B; Yin, Y Y; Tsutsumi, T; Hori, M; Han, Jeon G

2016-05-14

Control of the plasma densities and energies of the principal plasma species is crucial to induce modification of the plasma reactivity, chemistry, and film properties. This work presents a systematic and integrated approach to the low-temperature deposition of hydrogenated amorphous silicon nitride films looking into optimization and control of the plasma processes. Radiofrequency (RF) and ultrahigh frequency (UHF) power are combined to enhance significantly the nitrogen plasma and atomic-radical density to enforce their effect on film properties. This study presents an extensive investigation of the influence of combining radiofrequency (RF) and ultrahigh frequency (UHF) power as a power ratio (PR = RF : UHF), ranging from 4 : 0 to 0 : 4, on the compositional, structural, and optical properties of the synthesized films. The data reveal that DF power with a characteristic bi-Maxwellian electron energy distribution function (EEDF) is effectively useful for enhancing the ionization and dissociation of neutrals, which in turn helps in enabling high rate deposition with better film properties than that of SF operations. Utilizing DF PECVD, a wide-bandgap of ∼3.5 eV with strong photoluminescence features can be achieved only by using a high-density plasma and high nitrogen atom density at room temperature. The present work also proposes the suitability of the DF PECVD approach for industrial applications.

Interface properties of SiOxNy layer on Si prepared by atmospheric-pressure plasma oxidation-nitridation

PubMed Central

2013-01-01

SiOxNy films with a low nitrogen concentration (< 4%) have been prepared on Si substrates at 400°C by atmospheric-pressure plasma oxidation-nitridation process using O2 and N2 as gaseous precursors diluted in He. Interface properties of SiOxNy films have been investigated by analyzing high-frequency and quasistatic capacitance-voltage characteristics of metal-oxide-semiconductor capacitors. It is found that addition of N into the oxide increases both interface state density (Dit) and positive fixed charge density (Qf). After forming gas anneal, Dit decreases largely with decreasing N2/O2 flow ratio from 1 to 0.01 while the change of Qf is insignificant. These results suggest that low N2/O2 flow ratio is a key parameter to achieve a low Dit and relatively high Qf, which is effective for field effect passivation of n-type Si surfaces. PMID:23634872

Manual modification and plasma exposure of boron nitride ceramic to study Hall effect thruster plasma channel material erosion

NASA Astrophysics Data System (ADS)

Satonik, Alexander J.

Worn Hall effect thrusters (HET) show a variety of unique microstructures and elemental compositions in the boron nitride thruster channel walls. Worn thruster channels are typically created by running test thrusters in vacuum chambers for hundreds of hours. Studies were undertaken to manually modify samples of boron nitride without the use of a hall effect thruster. Samples were manually abraded with an abrasive blaster and sandpaper, in addition to a vacuum heater. Some of these samples were further exposed to a xenon plasma in a magnetron sputter device. Sandpaper and abrasive blaster tests were used to modify surface roughness values of the samples from 10,000 A to 150,000 A, matching worn thruster values. Vacuum heat treatments were performed on samples. These treatments showed the ability to modify chemical compositions of boron nitride samples, but not in a manner matching changes seen in worn thruster channels. Plasma erosion rate was shown to depend on the grade of the BN ceramic and the preparation of the surface prior to plasma exposure. Abraded samples were shown to erode 43% more than their pristine counterparts. Unique surface features and elemental compositions on the worn thruster channel samples were overwritten by new surface features on the ceramic grains. The microscope images of the ceramic surface show that the magnetron plasma source rounded the edges of the ceramic grains to closely match the worn HET surface. This effect was not as pronounced in studies of ion beam bombardment of the surface and appears to be a result of the quasi-neutral plasma environment.

Particle beam experiments for the analysis of reactive sputtering processes in metals and polymer surfaces

NASA Astrophysics Data System (ADS)

Corbella, Carles; Grosse-Kreul, Simon; Kreiter, Oliver; de los Arcos, Teresa; Benedikt, Jan; von Keudell, Achim

2013-10-01

A beam experiment is presented to study heterogeneous reactions relevant to plasma-surface interactions in reactive sputtering applications. Atom and ion sources are focused onto the sample to expose it to quantified beams of oxygen, nitrogen, hydrogen, noble gas ions, and metal vapor. The heterogeneous surface processes are monitored in situ by means of a quartz crystal microbalance and Fourier transform infrared spectroscopy. Two examples illustrate the capabilities of the particle beam setup: oxidation and nitriding of aluminum as a model of target poisoning during reactive magnetron sputtering, and plasma pre-treatment of polymers (PET, PP).

Gas-phase synthesis of semiconductor nanocrystals and its applications

NASA Astrophysics Data System (ADS)

Mandal, Rajib

Luminescent nanomaterials is a newly emerging field that provides challenges not only to fundamental research but also to innovative technology in several areas such as electronics, photonics, nanotechnology, display, lighting, biomedical engineering and environmental control. These nanomaterials come in various forms, shapes and comprises of semiconductors, metals, oxides, and inorganic and organic polymers. Most importantly, these luminescent nanomaterials can have different properties owing to their size as compared to their bulk counterparts. Here we describe the use of plasmas in synthesis, modification, and deposition of semiconductor nanomaterials for luminescence applications. Nanocrystalline silicon is widely known as an efficient and tunable optical emitter and is attracting great interest for applications in several areas. To date, however, luminescent silicon nanocrystals (NCs) have been used exclusively in traditional rigid devices. For the field to advance towards new and versatile applications for nanocrystal-based devices, there is a need to investigate whether these NCs can be used in flexible and stretchable devices. We show how the optical and structural/morphological properties of plasma-synthesized silicon nanocrystals (Si NCs) change when they are deposited on stretchable substrates made of polydimethylsiloxane (PDMS). Synthesis of these NCs was performed in a nonthermal, low-pressure gas phase plasma reactor. To our knowledge, this is the first demonstration of direct deposition of NCs onto stretchable substrates. Additionally, in order to prevent oxidation and enhance the luminescence properties, a silicon nitride shell was grown around Si NCs. We have demonstrated surface nitridation of Si NCs in a single step process using non?thermal plasma in several schemes including a novel dual-plasma synthesis/shell growth process. These coated NCs exhibit SiNx shells with composition depending on process parameters. While measurements including photoluminescence (PL), surface analysis, and defect identification indicate the shell is protective against oxidation compared to Si NCs without any shell growth. Gallium Nitride (GaN) is one of the most well-known semiconductor material and the industry standard for fabricating LEDs. The problem is that epitaxial growth of high-quality GaN requires costly substrates (e.g. sapphire), high temperatures, and long processing times. Synthesizing freestanding NCs of GaN, on the other hand, could enable these novel device morphologies, as the NCs could be incorporated into devices without the requirements imposed by epitaxial GaN growth. Synthesis of GaN NCs was performed using a fully gas-phase process. Different sizes of crystalline GaN nanoparticles were produced indicating versatility of this gas-phase process. Elemental analysis using X-ray photoelectron spectroscopy (XPS) indicated a possible nitrogen deficiency in the NCs; addition of secondary plasma for surface treatment indicates improving stoichiometric ratio and points towards a unique method for creating high-quality GaN NCs with ultimate alloying and doping for full-spectrum luminescence.

Thermally conductive tough flexible elastomers as composite of slide-ring materials and surface modified boron nitride particles via plasma in solution

NASA Astrophysics Data System (ADS)

Goto, Taku; Iida, Masaki; Tan, Helen; Liu, Chang; Mayumi, Koichi; Maeda, Rina; Kitahara, Koichi; Hatakeyama, Kazuto; Ito, Tsuyohito; Shimizu, Yoshiki; Yokoyama, Hideaki; Kimura, Kaoru; Ito, Kohzo; Hakuta, Yukiya; Terashima, Kazuo

2018-03-01

We have developed a thermally conductive flexible elastomer as a composite material with slide-ring (SR) materials and boron nitride (BN) particles surface-modified via plasma in solution. This composite shows excellent properties as a flexible insulator for thermal management. Surface modification of BN particles using plasma in solution increases the tensile strength, extension ratio at break, toughness, and rubber characteristics of the composites, compared to SR and non-modified BN, while the Young's modulus values are identical. Furthermore, the thermal conductivity also improved as a result of plasma surface modification.

Laser nitriding of iron: Nitrogen profiles and phases

NASA Astrophysics Data System (ADS)

Illgner, C.; Schaaf, P.; Lieb, K. P.; Schubert, E.; Queitsch, R.; Bergmann, H.-W.

1995-07-01

Armco iron samples were surface nitrided by irradiating them with pulses of an excimer laser in a nitrogen atmosphere. The resulting nitrogen depth profiles measured by Resonant Nuclear Reaction Analysis (RNRA) and the phase formation determined by Conversion Electron Mössbauer Spectroscopy (CEMS) were investigated as functions of energy density and the number of pulses. The nitrogen content of the samples was found to be independent of the number of pulses in a layer of 50 nm from the surface and to increase in depths exceeding 150 nm. The phase composition did not change with the number of pulses. The nitrogen content can be related to an enhanced nitrogen solubility based on high temperatures and high pressures due to the laser-induced plasma above the sample. With increasing pulse energy density, the phase composition changes towards phases with higher nitrogen contents. Nitrogen diffusion seems to be the limiting factor for the nitriding process.

Formation of carbon nitride — a novel hard coating

NASA Astrophysics Data System (ADS)

Chubaci, J. F. D.; Ogata, K.; Fujimoto, F.; Watanabe, S.; Biersack, J. P.

1996-08-01

Increasing efforts have been reported on the formation of carbon nitride. Vapor deposition and simultaneous ion bombardment from accelerators or plasmas (IBAD) proved to be a successful technique for the preparation of this material. In our preparation, the properties of the films were controlled by varying the nitrogen ion energy and the flux composition ratio {C}/{N}. The deposited films with high nitrogen incorporation ( {C}/{N} = 0.6 ˜ 0.7 ) and low implantation energies (< 1.0 keV) showed high Knoop hardnesses of up to 63 GPa. XPS and FT-IR measurements indicated a high fraction of triple bonded CN. X-ray diffraction showed an amorphous structure. Computer simulations by the dynamic TRIM code are used to study the formation parameters, nitrogen ion energy and {C}/{N} ratio. This turned on to be useful in understanding the formation process of the carbon nitride films grown on silicon wafers, fused silica and tungsten carbide substrates.

Substantial difference in target surface chemistry between reactive dc and high power impulse magnetron sputtering

NASA Astrophysics Data System (ADS)

Greczynski, G.; Mráz, S.; Schneider, J. M.; Hultman, L.

2018-02-01

The nitride layer formed in the target race track during the deposition of stoichiometric TiN thin films is a factor 2.5 thicker for high power impulse magnetron sputtering (HIPIMS), compared to conventional dc processing (DCMS). The phenomenon is explained using x-ray photoelectron spectroscopy analysis of the as-operated Ti target surface chemistry supported by sputter depth profiles, dynamic Monte Carlo simulations employing the TRIDYN code, and plasma chemical investigations by ion mass spectrometry. The target chemistry and the thickness of the nitride layer are found to be determined by the implantation of nitrogen ions, predominantly N+ and N2+ for HIPIMS and DCMS, respectively. Knowledge of this method-inherent difference enables robust processing of high quality functional coatings.

Characteristics of an Electron Cyclotron Resonance Plasma Source for the Production of Active Nitrogen Species in III-V Nitride Epitaxy

NASA Technical Reports Server (NTRS)

Meyyappan, Meyya; Arnold, James O. (Technical Monitor)

1997-01-01

A simple analysis is provided to determine the characteristics of an electron cyclotron resonance (ECR) plasma source for the generation of active nitrogen species in the molecular beam epitaxy of III-V nitrides. The effects of reactor geometry, pressure, power, and flow rate on the dissociation efficiency and ion flux are presented. Pulsing the input power is proposed to reduce the ion flux.

Tungsten nitride coatings obtained by HiPIMS as plasma facing materials for fusion applications

NASA Astrophysics Data System (ADS)

Tiron, Vasile; Velicu, Ioana-Laura; Porosnicu, Corneliu; Burducea, Ion; Dinca, Paul; Malinský, Petr

2017-09-01

In this work, tungsten nitride coatings with nitrogen content in the range of 19-50 at% were prepared by reactive multi-pulse high power impulse magnetron sputtering as a function of the argon and nitrogen mixture and further exposed to a deuterium plasma jet. The elemental composition, morphological properties and physical structure of the samples were investigated by Rutherford backscattering spectrometry, atomic force microscopy and X-ray diffraction. Deuterium implantation was performed using a deuterium plasma jet and its retention in nitrogen containing tungsten films was investigated using thermal desorption spectrometry. Deuterium retention and release behaviour strongly depend on the nitrogen content in the coatings and the films microstructure. All nitride coatings have a polycrystalline structure and retain a lower deuterium level than the pure tungsten sample. Nitrogen content in the films acts as a diffusion barrier for deuterium and leads to a higher desorption temperature, therefore to a higher binding energy.

Surface passivation of p-type Ge substrate with high-quality GeN{sub x} layer formed by electron-cyclotron-resonance plasma nitridation at low temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fukuda, Yukio; Otani, Yohei; Okamoto, Hiroshi

2011-09-26

We have investigated the effects of the formation temperature and postmetallization annealing (PMA) on the interface properties of GeN{sub x}/p-Ge fabricated by the plasma nitridation of Ge substrates using an electron-cyclotron-resonance-generated nitrogen plasma. The nitridation temperature is found to be a critical parameter in improving the finally obtained GeN{sub x}/Ge interface properties. The GeN{sub x}/Ge formed at room temperature and treated by PMA at 400 deg. C exhibits the best interface properties with an interface trap density of 1 x 10{sup 11 }cm{sup -2 }eV{sup -1}. The GeN{sub x}/Ge interface is unpinned and the Fermi level at the Ge surfacemore » can move from the valence band edge to the conduction band edge.« less

Soviet Developments in High Temperature Ceramics No. 1, January-December 1975

DTIC Science & Technology

1976-02-25

in microstructure and granulometric composition of silicon nitride in the process of hot pressing were studied by optical and electron micrographic...and on the laboratory-made a-alumina specimens^have shown that densely- sintered ceramics can be produced by a simplified process using a- Al -O...dusting of the powdered ceramic materials, spinel slurry deposition and subsequent fusion by a plasma jet traveling along the coated surface at

Direct spontaneous growth and interfacial structural properties of inclined GaN nanopillars on r-plane sapphire

DOE Office of Scientific and Technical Information (OSTI.GOV)

Adikimenakis, A.; Aretouli, K. E.; Tsagaraki, K.

2015-06-28

The spontaneous growth of GaN nanopillars (NPs) by direct plasma-assisted molecular beam epitaxy on nitridated r-plane sapphire substrates has been studied. The emanation of metal-polarity NPs from inside an a-plane nonpolar GaN film was found to depend on both the substrate nitridation and the growth conditions. The density of NPs increased with increasing the duration of the nitridation process and the power applied on the radio-frequency plasma source, as well as the III/V flux ratio, while variation of the first two parameters enhanced the roughness of the substrate's surface. Transmission electron microscopy (TEM) techniques were employed to reveal the structuralmore » characteristics of the NPs and their nucleation mechanism from steps on the sapphire surface and/or interfacial semipolar GaN nanocrystals. Lattice strain measurements showed a possible Al enrichment of the first 5–6 monolayers of the NPs. By combining cross-sectional and plan-view TEM observations, the three-dimensional model of the NPs was constructed. The orientation relationship and interfacial accommodation between the NPs and the nonpolar a-plane GaN film were also elucidated. The NPs exhibited strong and narrow excitonic emission, suggesting an excellent structural quality.« less

Process for depositing Cr-bearing layer

DOEpatents

Ellis, Timothy W.; Lograsso, Thomas A.; Eshelman, Mark A.

1995-05-09

A method of applying a Cr-bearing layer to a substrate, comprises introducing an organometallic compound, in vapor or solid powder form entrained in a carrier gas to a plasma of an inductively coupled plasma torch or device to thermally decompose the organometallic compound and contacting the plasma and the substrate to be coated so as to deposit the Cr-bearing layer on the substrate. A metallic Cr, Cr alloy or Cr compound such as chromium oxide, nitride and carbide can be provided on the substrate. Typically, the organometallic compound is introduced to an inductively coupled plasma torch that is disposed in ambient air so to thermally decompose the organometallic compound in the plasma. The plasma is directed at the substrate to deposit the Cr-bearing layer or coating on the substrate.

Process for depositing Cr-bearing layer

DOEpatents

Ellis, T.W.; Lograsso, T.A.; Eshelman, M.A.

1995-05-09

A method of applying a Cr-bearing layer to a substrate, comprises introducing an organometallic compound, in vapor or solid powder form entrained in a carrier gas to a plasma of an inductively coupled plasma torch or device to thermally decompose the organometallic compound and contacting the plasma and the substrate to be coated so as to deposit the Cr-bearing layer on the substrate. A metallic Cr, Cr alloy or Cr compound such as chromium oxide, nitride and carbide can be provided on the substrate. Typically, the organometallic compound is introduced to an inductively coupled plasma torch that is disposed in ambient air so to thermally decompose the organometallic compound in the plasma. The plasma is directed at the substrate to deposit the Cr-bearing layer or coating on the substrate. 7 figs.

Synthesis of TiN/a-Si3N4 thin film by using a Mather type dense plasma focus system

NASA Astrophysics Data System (ADS)

Hussain, T.; R., Ahmad; Khalid, N.; A. Umar, Z.; Hussnain, A.

2013-05-01

A 2.3 kJ Mather type pulsed plasma focus device was used for the synthesis of a TiN/a-Si3N4 thin film at room temperature. The film was characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The XRD pattern confirms the growth of polycrystalline TiN thin film. The XPS results indicate that the synthesized film is non-stoichiometric and contains titanium nitride, silicon nitride, and a phase of silicon oxy-nitride. The SEM and AFM results reveal that the surface of the synthesized film is quite smooth with 0.59 nm roughness (root-mean-square).

Etching Enhancement Followed by Nitridation on Low-k SiOCH Film in Ar/C5F10O Plasma

NASA Astrophysics Data System (ADS)

Miyawaki, Yudai; Shibata, Emi; Kondo, Yusuke; Takeda, Keigo; Kondo, Hiroki; Ishikawa, Kenji; Okamoto, Hidekazu; Sekine, Makoto; Hori, Masaru

2013-02-01

The etching rates of low-dielectric-constant (low-k), porous SiOCH (p-SiOCH) films were increased by nitrogen-added Ar/C5F10O plasma etching in dual-frequency (60 MHz/2 MHz)-excited parallel plate capacitively coupled plasma. Previously, perfluoropropyl vinyl ether [C5F10O] provided a very high density of CF3+ ions [Nagai et al.: Jpn. J. Appl. Phys. 45 (2006) 7100]. Surface nitridation on the p-SiOCH surface exposed to Ar/N2 plasma led to the etching of larger amounts of p-SiOCH in Ar/C5F10O plasma, which depended on the formation of bonds such as =C(sp2)=N(sp2)- and -C(sp)≡N(sp).

Incorporation of low energy activated nitrogen onto HOPG surface: Chemical states and thermal stability studies by in-situ XPS and Raman spectroscopy

NASA Astrophysics Data System (ADS)

Chandran, Maneesh; Shasha, Michal; Michaelson, Shaul; Hoffman, Alon

2016-09-01

In this paper we report the chemical states analysis of activated nitrogen incorporated highly oriented pyrolytic graphite (HOPG) surface under well-controlled conditions. Nitrogen incorporation is carried out by two different processes: an indirect RF nitrogen plasma and low energy (1 keV) N2+ implantation. Bonding configuration, concentration and thermal stability of the incorporated nitrogen species by aforesaid processes are systematically compared by in-situ X-ray photoelectron spectroscopy (XPS). Relatively large concentration of nitrogen is incorporated onto RF nitride HOPG surface (16.2 at.%), compared to N2+ implanted HOPG surface (7.7 at.%). The evolution of N 1s components (N1, N2, N3) with annealing temperature is comprehensively discussed, which indicates that the formation and reorganization of local chemical bonding states are determined by the process of nitridation and not by the prior chemical conditioning (i.e., amorphization or hydrogenation) of the HOPG surface. A combined XPS and Raman spectroscopy studies revealed that N2+ implantation process resulted in a high level of defects to the HOPG surface, which cannot be annealed-out by heat treatment up to 1000 °C. On the other hand, the RF nitrogen plasma process did not produce a high level of surface defects, while incorporating nearly the same amount of stable nitrogen species.

Slurry Erosion Studies on Surface Modified 13Cr-4Ni Steels: Effect of Angle of Impingement and Particle Size

NASA Astrophysics Data System (ADS)

Manisekaran, T.; Kamaraj, M.; Sharrif, S. M.; Joshi, S. V.

2007-10-01

Hydroturbine steels, such as 13Cr-4Ni martensitic steels, are generally subjected to heavy-erosive wear and loss of efficiency due to solid particulate entrainment in the water. Surface-modified steels have proven to give better performance in terms of erosive wear resistance. In the present study, an attempt is made to investigate the effect of angle of impingement and particle size on slurry-jet erosion behavior of pulsed plasma nitrided and laser hardened 13Cr-4Ni steels. Laser hardening process has shown good performance at all angles of impingement due to martensitic transformation of retained austenite. Plastic deformation mode of material removal was also an evident feature of all laser-hardened surface damage locations. However, pulsed-plasma nitrided steels have exhibited chip formation and micro-cutting mode of erosive wear. Erosion with 150-300 μm size was twice compared to 150 μm size slurry particulates.

Comparative study on nitridation and oxidation plasma interface treatment for AlGaN/GaN MIS-HEMTs with AlN gate dielectric

NASA Astrophysics Data System (ADS)

Zhu, Jie-Jie; Ma, Xiao-Hua; Hou, Bin; Chen, Li-Xiang; Zhu, Qing; Hao, Yue

2017-02-01

This paper demonstrated the comparative study on interface engineering of AlN/AlGaN/GaN metal-insulator-semiconductor high-electron-mobility transistors (MIS-HEMTs) by using plasma interface pre-treatment in various ambient gases. The 15 nm AlN gate dielectric grown by plasma-enhanced atomic layer deposition significantly suppressed the gate leakage current by about two orders of magnitude and increased the peak field-effect mobility by more than 50%. NH3/N2 nitridation plasma treatment (NPT) was used to remove the 3 nm poor-quality interfacial oxide layer and N2O/N2 oxidation plasma treatment (OPT) to improve the quality of interfacial layer, both resulting in improved dielectric/barrier interface quality, positive threshold voltage (V th) shift larger than 0.9 V, and negligible dispersion. In comparison, however, NPT led to further decrease in interface charges by 3.38 × 1012 cm-2 and an extra positive V th shift of 1.3 V. Analysis with fat field-effect transistors showed that NPT resulted in better sub-threshold characteristics and transconductance linearity for MIS-HEMTs compared with OPT. The comparative study suggested that direct removing the poor interfacial oxide layer by nitridation plasma was superior to improving the quality of interfacial layer by oxidation plasma for the interface engineering of GaN-based MIS-HEMTs.

Atomic Layer Deposition of Wet-Etch Resistant Silicon Nitride Using Di(sec-butylamino)silane and N2 Plasma on Planar and 3D Substrate Topographies.

PubMed

Faraz, Tahsin; van Drunen, Maarten; Knoops, Harm C M; Mallikarjunan, Anupama; Buchanan, Iain; Hausmann, Dennis M; Henri, Jon; Kessels, Wilhelmus M M

2017-01-18

The advent of three-dimensional (3D) finFET transistors and emergence of novel memory technologies place stringent requirements on the processing of silicon nitride (SiN x ) films used for a variety of applications in device manufacturing. In many cases, a low temperature (<400 °C) deposition process is desired that yields high quality SiN x films that are etch resistant and also conformal when grown on 3D substrate topographies. In this work, we developed a novel plasma-enhanced atomic layer deposition (PEALD) process for SiN x using a mono-aminosilane precursor, di(sec-butylamino)silane (DSBAS, SiH 3 N( s Bu) 2 ), and N 2 plasma. Material properties have been analyzed over a wide stage temperature range (100-500 °C) and compared with those obtained in our previous work for SiN x deposited using a bis-aminosilane precursor, bis(tert-butylamino)silane (BTBAS, SiH 2 (NH t Bu) 2 ), and N 2 plasma. Dense films (∼3.1 g/cm 3 ) with low C, O, and H contents at low substrate temperatures (<400 °C) were obtained on planar substrates for this process when compared to other processes reported in the literature. The developed process was also used for depositing SiN x films on high aspect ratio (4.5:1) 3D trench nanostructures to investigate film conformality and wet-etch resistance (in dilute hydrofluoric acid, HF/H 2 O = 1:100) relevant for state-of-the-art device architectures. Film conformality was below the desired levels of >95% and attributed to the combined role played by nitrogen plasma soft saturation, radical species recombination, and ion directionality during SiN x deposition on 3D substrates. Yet, very low wet-etch rates (WER ≤ 2 nm/min) were observed at the top, sidewall, and bottom trench regions of the most conformal film deposited at low substrate temperature (<400 °C), which confirmed that the process is applicable for depositing high quality SiN x films on both planar and 3D substrate topographies.

The Automated Array Assembly Task of the Low-cost Silicon Solar Array Project, Phase 2

NASA Technical Reports Server (NTRS)

Coleman, M. G.; Grenon, L.; Pastirik, E. M.; Pryor, R. A.; Sparks, T. G.

1978-01-01

An advanced process sequence for manufacturing high efficiency solar cells and modules in a cost-effective manner is discussed. Emphasis is on process simplicity and minimizing consumed materials. The process sequence incorporates texture etching, plasma processes for damage removal and patterning, ion implantation, low pressure silicon nitride deposition, and plated metal. A reliable module design is presented. Specific process step developments are given. A detailed cost analysis was performed to indicate future areas of fruitful cost reduction effort. Recommendations for advanced investigations are included.

Enhanced saturation of sputtered amorphous SiN film frameworks using He- and Ne-Penning effects

NASA Astrophysics Data System (ADS)

Sugimoto, Iwao; Nakano, Satoko; Kuwano, Hiroki

1994-06-01

Optical emission spectroscopy reveals that helium and neon gases enhance the nitridation reactivity of the nitrogen plasma by Penning effects during magnetron sputtering of the silicon target. These excited nitrogen plasmas promote the saturation of frameworks of the resultant silicon nitride films. X-ray photoelectron spectroscopy, electron spin resonance, and x-ray diffraction analyses provide insight into the structure of these films, and thermal desorption mass spectroscopy reveals the behavior of volatile species in these films.

Fabrication of AlN/BN bishell hollow nanofibers by electrospinning and atomic layer deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haider, Ali; Kayaci, Fatma; Uyar, Tamer

2014-09-01

Aluminum nitride (AlN)/boron nitride (BN) bishell hollow nanofibers (HNFs) have been fabricated by successive atomic layer deposition (ALD) of AlN and sequential chemical vapor deposition (CVD) of BN on electrospun polymeric nanofibrous template. A four-step fabrication process was utilized: (i) fabrication of polymeric (nylon 6,6) nanofibers via electrospinning, (ii) hollow cathode plasma-assisted ALD of AlN at 100 °C onto electrospun polymeric nanofibers, (iii) calcination at 500 °C for 2 h in order to remove the polymeric template, and (iv) sequential CVD growth of BN at 450 °C. AlN/BN HNFs have been characterized for their chemical composition, surface morphology, crystal structure, and internal nanostructuremore » using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, and selected area electron diffraction. Measurements confirmed the presence of crystalline hexagonal BN and AlN within the three dimensional (3D) network of bishell HNFs with relatively low impurity content. In contrast to the smooth surface of the inner AlN layer, outer BN coating showed a highly rough 3D morphology in the form of BN nano-needle crystallites. It is shown that the combination of electrospinning and plasma-assisted low-temperature ALD/CVD can produce highly controlled multi-layered bishell nitride ceramic hollow nanostructures. While electrospinning enables easy fabrication of nanofibrous template, self-limiting reactions of plasma-assisted ALD and sequential CVD provide control over the wall thicknesses of AlN and BN layers with sub-nanometer accuracy.« less

Hafnium nitride buffer layers for growth of GaN on silicon

DOEpatents

Armitage, Robert D.; Weber, Eicke R.

2005-08-16

Gallium nitride is grown by plasma-assisted molecular-beam epitaxy on (111) and (001) silicon substrates using hafnium nitride buffer layers. Wurtzite GaN epitaxial layers are obtained on both the (111) and (001) HfN/Si surfaces, with crack-free thickness up to 1.2 {character pullout}m. However, growth on the (001) surface results in nearly stress-free films, suggesting that much thicker crack-free layers could be obtained.

Failure Mechanisms for III-Nitride HEMT Devices

DTIC Science & Technology

2013-11-19

rf plasma-assisted molecular beam epitaxy on freestanding GaN substrates, J. Cryst. Growth 380, 14-17 (2013). ii) Conference presentations (Invited...1 eFinal Report – AOARD Grant FA-2386-11-1-4107 Failure Mechanisms for III-nitride HEMT devices 19 November 2013 Principal Investigators: Martha...aspects of III-nitride HEMT materials and devices. Energy-filtered imaging of unstressed and stressed Ni/Au-gated AlGaN/GaN HEMTs indicated that

Research on Nitride Thin Films, Advanced Plasma Diagnostics, and Charged-Particle Processes

DTIC Science & Technology

2006-07-01

Additionally, these components are being placed closer to the point of use--requiring that they operate in extreme temperature environments ...reasons for component failure. To operate in extreme temperature environments , electronic and electrical components must withstand higher ambient...hybrid and plug-in hybrid-powered automobiles, heart defibrillators , and industrial equipment will benefit from a new generation of capacitors. High

Effect of plasma nitriding on the structural stability and hydrogen absorption capability of Pd-coated Nb during thermal treatment

NASA Astrophysics Data System (ADS)

Ohtsu, Naofumi; Kozuka, Taro; Shibata, Yuga; Yamane, Misao

2017-11-01

Plasma nitriding was explored for improving the thermal stability of a composite hydrogen permeable membrane comprising a Pd coating on Nb substrate. A NbN intermediate layer was formed on the Nb substrate, and the progress of interdiffusion and deterioration of hydrogen absorption behavior after a thermal treatment at 573 and 773 K, respectively, were investigated. The intermediate layer significantly suppressed the interdiffusion between the coating and the substrate. Furthermore, an increase in the NbN concentration of the intermediate layer enhanced the suppression efficiency. However, the hydrogen permeability of the intermediate layer was significantly low, and hence, an increase in NbN concentration further decreased the hydrogen permeability. We concluded that the nitride layer with a high NbN content was unsuitable as an intermediate layer owing to its low hydrogen permeability, while the partial nitride layer with a low NbN content was inefficient in suppressing the interdiffusion.

New frontiers of atomic layer etching

NASA Astrophysics Data System (ADS)

Sherpa, Sonam D.; Ranjan, Alok

2018-03-01

Interest in atomic layer etching (ALE) has surged recently because it offers several advantages over continuous or quasicontinuous plasma etching. These benefits include (1) independent control of ion energy, ion flux, and radical flux, (2) flux-independent etch rate that mitigates the iso-dense loading effects, and (3) ability to control the etch rate with atomic or nanoscale precision. In addition to these benefits, we demonstrate an area-selective etching for maskless lithography as a new frontier of ALE. In this paper, area-selective etching refers to the confinement of etching into the specific areas of the substrate. The concept of area-selective etching originated during our studies on quasi-ALE of silicon nitride which consists of sequential exposure of silicon nitride to hydrogen and fluorinated plasma. The findings of our studies reported in this paper suggest that it may be possible to confine the etching into specific areas of silicon nitride without using any mask by replacing conventional hydrogen plasma with a localized source of hydrogen ions.

Thermal and Kerr nonlinear properties of plasma-deposited silicon nitride/ silicon dioxide waveguides.

PubMed

Ikeda, Kazuhiro; Saperstein, Robert E; Alic, Nikola; Fainman, Yeshaiahu

2008-08-18

We introduce and present experimental evaluations of loss and nonlinear optical response in a waveguide and an optical resonator, both implemented with a silicon nitride/ silicon dioxide material platform prepared by plasma-enhanced chemical vapor deposition with dual frequency reactors that significantly reduce the stress and the consequent loss of the devices. We measure a relatively small loss of approximately 4dB/cm in the waveguides. The fabricated ring resonators in add-drop and all-pass arrangements demonstrate quality factors of Q=12,900 and 35,600. The resonators are used to measure both the thermal and ultrafast Kerr nonlinearities. The measured thermal nonlinearity is larger than expected, which is attributed to slower heat dissipation in the plasma-deposited silicon dioxide film. The n2 for silicon nitride that is unknown in the literature is measured, for the first time, as 2.4 x 10(-15)cm(2)/W, which is 10 times larger than that for silicon dioxide.

Low-temperature formation of c-axis-oriented aluminum nitride thin films by plasma-assisted reactive pulsed-DC magnetron sputtering

NASA Astrophysics Data System (ADS)

Takenaka, Kosuke; Satake, Yoshikatsu; Uchida, Giichiro; Setsuhara, Yuichi

2018-01-01

The low-temperature formation of c-axis-oriented aluminum nitride thin films was demonstrated by plasma-assisted reactive pulsed-DC magnetron sputtering. The effects of the duty cycle at the pulsed-DC voltage applied to the Al target on the properties of AlN films formed via inductively coupled plasma (ICP)-enhanced pulsed-DC magnetron sputtering deposition were investigated. With decreasing duty cycle at the target voltage, the peak intensity of AlN(0002) increased linearly. The surface roughness of AlN films decreased since there was an increase in film density owing to the impact of energetic ions on the films together with the enhancement of nitriding associated with the relative increase in N radical flux. The improvement of both the crystallinity and surface morphology of AlN films at low temperatures is considered to be caused by the difference between the relative flux values of ions and sputtered atoms.

Redeposition in plasma-assisted atomic layer deposition: Silicon nitride film quality ruled by the gas residence time

DOE Office of Scientific and Technical Information (OSTI.GOV)

Knoops, Harm C. M., E-mail: h.c.m.knoops@tue.nl, E-mail: w.m.m.kessels@tue.nl; Oxford Instruments Plasma Technology, North End, Bristol BS49 4AP; Peuter, K. de

2015-07-06

The requirements on the material properties and growth control of silicon nitride (SiN{sub x}) spacer films in transistors are becoming ever more stringent as scaling of transistor structures continues. One method to deposit high-quality films with excellent control is atomic layer deposition (ALD). However, depositing SiN{sub x} by ALD has turned out to be very challenging. In this work, it is shown that the plasma gas residence time τ is a key parameter for the deposition of SiN{sub x} by plasma-assisted ALD and that this parameter can be linked to a so-called “redeposition effect”. This previously ignored effect, which takesmore » place during the plasma step, is the dissociation of reaction products in the plasma and the subsequent redeposition of reaction-product fragments on the surface. For SiN{sub x} ALD using SiH{sub 2}(NH{sup t}Bu){sub 2} as precursor and N{sub 2} plasma as reactant, the gas residence time τ was found to determine both SiN{sub x} film quality and the resulting growth per cycle. It is shown that redeposition can be minimized by using a short residence time resulting in high-quality films with a high wet-etch resistance (i.e., a wet-etch rate of 0.5 nm/min in buffered HF solution). Due to the fundamental nature of the redeposition effect, it is expected to play a role in many more plasma-assisted ALD processes.« less

Electron impact ionization in plasma technologies; studies on atomic boron and BN molecule

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joshi, Foram M., E-mail: foram29@gmail.com; Joshipura, K. N., E-mail: knjoshipura22@gmail.com; Chaudhari, Asha S., E-mail: ashaschaudhari@gmail.com

2016-05-06

Electron impact ionization plays important role in plasma technologies. Relevant cross sections on atomic boron are required to understand the erosion processes in fusion experiments. Boronization of plasma exposed surfaces of tokomaks has proved to be an effective way to produce very pure fusion plasmas. This paper reports comprehensive theoretical investigations on electron scattering with atomic Boron and Boron Nitride in solid phases. Presently we determine total ionization cross-section Q{sub ion} and the summed-electronic excitation cross section ΣQ{sub exc} in a standard quantum mechanical formalism called SCOP and CSP-ic methods. Our calculated cross sections are examined as functions of incidentmore » electron energy along with available comparisons.« less

Silicon cells made by self-aligned selective-emitter plasma-etchback process

DOEpatents

Ruby, Douglas S.; Schubert, William K.; Gee, James M.; Zaidi, Saleem H.

2000-01-01

Photovoltaic cells and methods for making them are disclosed wherein the metallized grids of the cells are used to mask portions of cell emitter regions to allow selective etching of phosphorus-doped emitter regions. The preferred etchant is SF.sub.6 or a combination of SF.sub.6 and O.sub.2. This self-aligned selective etching allows for enhanced blue response (versus cells with uniform heavy doping of the emitter) while preserving heavier doping in the region beneath the gridlines needed for low contact resistance. Embodiments are disclosed for making cells with or without textured surfaces. Optional steps include plasma hydrogenation and PECVD nitride deposition, each of which are suited to customized applications for requirements of given cells to be manufactured. The techniques disclosed could replace expensive and difficult alignment methodologies used to obtain selectively etched emitters, and they may be easily integrated with existing plasma processing methods and techniques of the invention may be accomplished in a single plasma-processing chamber.

Low temperature synthesis of silicon nitride thin films deposited by VHF/RF PECVD for gas barrier application

NASA Astrophysics Data System (ADS)

Lee, Jun S.; Shin, Kyung S.; Sahu, B. B.; Han, Jeon G.

2015-09-01

In this work, silicon nitride (SiNx) thin films were deposited on polyethylene terephthalate (PET) substrates as barrier layers by plasma enhanced chemical vapor deposition (PECVD) system. Utilizing a combination of very high-frequency (VHF 40.68 MHz) and radio-frequency (RF 13.56 MHz) plasmas it was possible to adopt PECVD deposition at low-temperature using the precursors: Hexamethyldisilazane (HMDSN) and nitrogen. To investigate relationship between film properties and plasma properties, plasma diagnostic using optical emission spectroscopy (OES) was performed along with the film analysis using Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). OES measurements show that there is dominance of the excited N2 and N2+ emissions with increase in N2 dilution, which has a significant impact on the film properties. It was seen that all the deposited films contains mainly silicon nitride with a small content of carbon and no signature of oxygen. Interestingly, upon air exposure, films have shown the formation of Si-O bonds in addition to the Si-N bonds. Measurements and analysis reveals that SiNx films deposited with high content of nitrogen with HMDSN plasma can have lower gas barrier properties as low as 7 . 3 ×10-3 g/m2/day. Also at Chiang Mai University.

Systematic Study of p-type Doping and Related Defects in III-Nitrides: Pathway toward a Nitride HBT

DTIC Science & Technology

2012-11-20

InGaN growth where an intermediate regime does not exist.40 Considering GaN molecular - beam epitaxy (MBE) growth phase diagrams such as those...1009 (2007). 44 S. D. Burnham, Improved Understanding and Control of Magnesium-Doped Gallium Nitride by Plasma Assisted Molecular Beam Epitaxy , in...reported using a modified form of molecular beam epitaxy (MBE) called Metal-Modulated Epitaxy (MME).11, 12 The details of this shuttered technique

Very low temperature materials and self-alignment technology for amorphous hydrated silicon thin film transistors fabricated on transparent large area plastic substrates

NASA Astrophysics Data System (ADS)

Yang, Chien-Sheng

The purpose of this research has been to (1) explore materials prepared using plasma enhanced chemical vapor deposition (PECVD) at 110sp°C for amorphous silicon thin film transistors (TFT's) fabricated on low temperature compatible, large area flexible polyethylene terephthalate (PET) substrates, and (2) develop full self-alignment technology using selective area n+ PECVD for source/drain contacts of amorphous silicon TFT's. For item (1), silicon nitride films, as gate dielectrics of TFT's, were deposited using SiHsb4+NHsb3, SiHsb4+NHsb3+Nsb2, SiHsb4+NHsb3+He, or SiHsb4+NHsb3+Hsb2 gases. Good quality silicon nitride films can be deposited using a SiHsb4+NHsb3 gas with high NHsb3/SiHsb4 ratios, or using a SiHsb4+NHsb3+Nsb2 gas with moderate NHsb3/SiHsb4 ratios. A chemical model was proposed to explain the Nsb2 dilution effect. This model includes calculations of (a) the electron energy distribution function in a plasma, (b) rate constants of electron impact dissociation, and (3) the (NHsbx) / (SiHsby) ratio in a plasma. The Nsb2 dilution was shown to have a effect of shifting the electron energy distribution into high energy, thus enhancing the (NHsbx) / (SiHsbyrbrack ratio in a plasma and promoting the deposition of N-rich silicon nitride films, which leads to decreased trap state density and a shift in trap state density to deeper in the gap. Amorphous silicon were formed successfully at 110sp°C on large area glass and plastic(PET) substrates. Linear mobilities are 0.33 and 0.12 cmsp2/Vs for TFT's on glass and plastic substrates, respectively. ON/OFF current ratios exceed 10sp7 for TFT's on glass and 10sp6 for TFT's on PET. For item (2), a novel full self-alignment process was developed for amorphous silicon TFT's. This process includes (1) back-exposure using the bottom gate metal as the mask, and (2) selective area n+ micro-crystalline silicon PECVD for source/drain contacts of amorphous silicon TFT's. TFT's fabricated using the full self-alignment process showed linear mobilities ranging from 0.5 to 1.0 cmsp2/Vs.

Method for surface passivation and protection of cadmium zinc telluride crystals

DOEpatents

Mescher, Mark J.; James, Ralph B.; Schlesinger, Tuviah E.; Hermon, Haim

2000-01-01

A method for reducing the leakage current in CZT crystals, particularly Cd.sub.1-x Zn.sub.x Te crystals (where x is greater than equal to zero and less than or equal to 0.5), and preferably Cd.sub.0.9 Zn.sub.0.1 Te crystals, thereby enhancing the ability of these crystal to spectrally resolve radiological emissions from a wide variety of radionuclides. Two processes are disclosed. The first method provides for depositing, via reactive sputtering, a silicon nitride hard-coat overlayer which provides significant reduction in surface leakage currents. The second method enhances the passivation by oxidizing the CZT surface with an oxygen plasma prior to silicon nitride deposition without breaking the vacuum state.

PECVD silicon-rich nitride and low stress nitride films mechanical characterization using membrane point load deflection

NASA Astrophysics Data System (ADS)

Bagolini, Alvise; Picciotto, Antonino; Crivellari, Michele; Conci, Paolo; Bellutti, Pierluigi

2016-02-01

An analysis of the mechanical properties of plasma enhanced chemical vapor (PECVD) silicon nitrides is presented, using micro fabricated silicon nitride membranes under point load deflection. The membranes are made of PECVD silicon-rich nitride and low stress nitride films. The mechanical performance of the bended membranes is examined both with analytical models and finite element simulation in order to extract the elastic modulus and residual stress values. The elastic modulus of low stress silicon nitride is calculated using stress free analytical models, while for silicon-rich silicon nitride and annealed low stress silicon nitride it is estimated with a pre-stressed model of point-load deflection. The effect of annealing both in nitrogen and hydrogen atmosphere is evaluated in terms of residual stress, refractive index and thickness variation. It is demonstrated that a hydrogen rich annealing atmosphere induces very little change in low stress silicon nitride. Nitrogen annealing effects are measured and shown to be much higher in silicon-rich nitride than in low stress silicon nitride. An estimate of PECVD silicon-rich nitride elastic modulus is obtained in the range between 240-320 GPa for deposited samples and 390 GPa for samples annealed in nitrogen atmosphere. PECVD low stress silicon nitride elastic modulus is estimated to be 88 GPa as deposited and 320 GPa after nitrogen annealing.

Method of chemical vapor deposition of boron nitride using polymeric cyanoborane

DOEpatents

Maya, Leon

1994-01-01

Polymeric cyanoborane is volatilized, decomposed by thermal or microwave plasma energy, and deposited on a substrate as an amorphous film containing boron, nitrogen and carbon. Residual carbon present in the film is removed by ammonia treatment at an increased temperature, producing an adherent, essentially stoichiometric boron nitride film.

Structure and hemocompatibility of nanocrystalline titanium nitride produced under glow-discharge conditions

NASA Astrophysics Data System (ADS)

Sowińska, Agnieszka; Czarnowska, Elżbieta; Tarnowski, Michał; Witkowska, Justyna; Wierzchoń, Tadeusz

2018-04-01

Significant efforts are being made towards developing novel antithrombotic materials. The purpose of the presented study was to characterize two variants of nitrided surface layers produced on alloy Ti-6Al-4V in different areas of low-temperature plasma - at the plasma potential (TiNp) or at the cathode potential (TiNc). The layers were characterized in terms of their microstructure, surface topography and wettability, and platelet response to the environment of different pH. The produced layers were of the TiN + Ti2N + αTiN-type, but the layer produced at the plasma potential was thinner, smoother and had lower surface free energy compared with that produced at the cathode potential. Biological evaluation demonstrated more fibrinogen buildup, less platelet adhesion and aggregation, and fewer strongly activated platelets on the TiNp surface compared with those parameters on the TiNc surface and on the titanium alloy in its initial state. Interestingly, both surface types were significantly resistant to fibrinogen adsorption and platelet adhesion in the environment of lower pH. In conclusion, the nitrided surface layer produced at the plasma potential is a promising material and this basic information is critical for further development of hemocompatible materials.

X-Ray Photoelectron Spectroscopy and Ultrahigh Vacuum Contactless Capacitance-Voltage Characterization of Novel Oxide-Free InP Passivation Process Using a Silicon Surface Quantum Well

NASA Astrophysics Data System (ADS)

Takahashi, Hiroshi; Hashizume, Tamotsu; Hasegawa, Hideki

1999-02-01

In order to understand and optimize a novel oxide-free InP passivation process using a silicon surface quantum well, a detailed in situ X-ray photoelectron spectroscopy (XPS) and ultrahigh vacuum (UHV) contactless capacitance-voltage (C-V) study of the interface was carried out. Calculation of quantum levels in the silicon quantum well was performed on the basis of the band lineup of the strained Si3N4/Si/InP interface and the result indicated that the interface should become free of gap states when the silicon layer thickness is below 5 Å. Experimentally, such a delicate Si3N4/Si/InP structure was realized by partial nitridation of a molecular beam epitaxially (MBE) grown pseudomorphic silicon layer using an electron cyclotron resonance (ECR) N2 plasma. The progress of nitridation was investigated in detail by angle-resolved XPS. A newly developed UHV contactless C-V method realized in situ characterization of surface electronic properties of InP at each processing step for passivation. It was found that the interface state density decreased substantially into the 1010 cm-2 eV-1 range by optimizing the nitridation process of the silicon layer. It was concluded that both the surface bond termination and state removal by quantum confinement are responsible for the NSS reduction.

MBE growth of nitride-arsenides for long wavelength opto-electronics

NASA Astrophysics Data System (ADS)

Spruytte, Sylvia Gabrielle

2001-07-01

Until recently, the operating wavelength of opto-electronic devices on GaAs has been limited to below 1 mum due to the lack of III-V materials with close lattice match to GaAs that have a bandgap below 1.24 eV. To enable devices operating at 1.3 mum on GaAs, MBE growth of a new III-V material formed by adding small amounts of nitrogen to InGaAs was developed. The growth of group III-nitride-arsenides (GaInNAs) is complicated by the divergent properties of the alloy constituents and the difficulty of generating a reactive nitrogen species. Nitride-arsenide materials are grown by molecular beam epitaxy (MBE) using a radio frequency (rf) nitrogen plasma source. The plasma conditions that maximize the amount of atomic nitrogen versus molecular nitrogen are determined using the emission spectrum of the plasma. To avoid phase segregation, nitride-arsenides must be grown at relatively low temperatures and high arsenic overpressures. It is shown that the group III growth rate controls the nitrogen concentration in the film. Absorption measurements allow the establishment of a range of GaInNAs alloys yielding 1.3 mum emission. The optical properties of GaInNAs and GaNAs quantum wells (QWs) are investigated with photoluminescence (PL) measurements. The peak PL intensity increases and peak wavelength shifts to shorter wavelengths when annealing. The increase in luminescence efficiency results from a decrease in non-radiative recombination centers. As the impurity concentration in the GaInNAs films is low, crystal defects associated with nitrogen incorporation were investigated and improvements in crystal quality after anneal were observed. Nuclear reaction channeling measurements show that as-grown nitride-arsenides contain a considerable amount of interstitial nitrogen and that a substantial fraction of the non-substitutional nitrogen disappears during anneal. Secondary ion mass spectroscopy depth profiling on GaInNAs quantum wells shows that during anneal, the nitrogen diffusion is more pronounced than indium diffusion, hence nitrogen diffusion is also the major cause of the shift during the anneal process of GaInNAs QWs. To limit nitrogen diffusion, the GaInNAs QWs were inserted between GaAsN barriers. This also resulted in longer wavelength emission due to decreased carrier confinement energy. This new active region resulted in devices emitting at 1.3 mum.

High temperature solar energy absorbing surfaces

DOEpatents

Schreyer, J.M.; Schmitt, C.R.; Abbatiello, L.A.

A solar collector having an improved coating is provided. The coating is a plasma-sprayed coating comprising a material having a melting point above 500/sup 0/C at which it is stable and selected from the group of boron carbide, boron nitride, metals and metal oxides, nitrides, carbides, borides, and silicates. The coatings preferably have a porosity of about 15 to 25% and a thickness of less than 200 micrometers. The coatings can be provided by plasma-spraying particles having a mean diameter of about 10 to 200 micrometers.

On the S-phase formation and the balanced plasma nitriding of austenitic-ferritic super duplex stainless steel

NASA Astrophysics Data System (ADS)

de Oliveira, Willian R.; Kurelo, Bruna C. E. S.; Ditzel, Dair G.; Serbena, Francisco C.; Foerster, Carlos E.; de Souza, Gelson B.

2018-03-01

The different physical responses of austenite (γ) and ferrite (α) iron structures upon nitriding result in technical challenges to the uniform modification of α-γ materials, as the super duplex stainless steel (SDSS). The effects of voltage (7-10 kV), frequency and pulse width on the nitrogen plasma immersion ion implantation of SDSS (α ∼ 56%, γ ∼ 44%) were investigated, correlated with structural, morphological and mechanical analyses. By controlling the treatment power, temperatures ranged from 292 °C to 401 °C. Despite the overall increase in hardness for any of the employed parameters (from ∼6 GPa to ∼15 GPa), the structure of individual grains was strikingly dissimilar at the same temperatures, depending on the energetic conditions of implantation. Modified-α grains containing iron nitrides (ε-Fe2-3N, γ‧ -Fe4N) presented intense brittleness, whereas the expanded phase γN (S-phase) laid principally in modified-γ grains, exhibiting ductile-like deformation features and thicker layers. The γN was the dominant phase in both α-γ grains at ∼401 °C, providing them with balanced structure and mechanical behavior. These phenomena corroborate with γN as mediator of the process, through a mechanism involving the nitrogen-promoted ferrite to austenite conversion and nitrides dissolution at high temperatures. An approximately linear correlation of the γN content with respect to the ion energy per pulse was demonstrated, which properly embodies limiting effects to the treatment. This can be a parameter for the α-γ steel surface modification, consisting in a better adjustment to obtain more precise control along with temperature.

Bismuth Passivation Technique for High-Resolution X-Ray Detectors

NASA Technical Reports Server (NTRS)

Chervenak, James; Hess, Larry

2013-01-01

The Athena-plus team requires X-ray sensors with energy resolution of better than one part in 3,000 at 6 keV X-rays. While bismuth is an excellent material for high X-ray stopping power and low heat capacity (for large signal when an X-ray is stopped by the absorber), oxidation of the bismuth surface can lead to electron traps and other effects that degrade the energy resolution. Bismuth oxide reduction and nitride passivation techniques analogous to those used in indium passivation are being applied in a new technique. The technique will enable improved energy resolution and resistance to aging in bismuth-absorber-coupled X-ray sensors. Elemental bismuth is lithographically integrated into X-ray detector circuits. It encounters several steps where the Bi oxidizes. The technology discussed here will remove oxide from the surface of the Bi and replace it with nitridized surface. Removal of the native oxide and passivating to prevent the growth of the oxide will improve detector performance and insulate the detector against future degradation from oxide growth. Placing the Bi coated sensor in a vacuum system, a reduction chemistry in a plasma (nitrogen/hydrogen (N2/H2) + argon) is used to remove the oxide and promote nitridization of the cleaned Bi surface. Once passivated, the Bi will perform as a better X-ray thermalizer since energy will not be trapped in the bismuth oxides on the surface. A simple additional step, which can be added at various stages of the current fabrication process, can then be applied to encapsulate the Bi film. After plasma passivation, the Bi can be capped with a non-diffusive layer of metal or dielectric. A non-superconducting layer is required such as tungsten or tungsten nitride (WNx).

Correlation of film density and wet etch rate in hydrofluoric acid of plasma enhanced atomic layer deposited silicon nitride

DOE Office of Scientific and Technical Information (OSTI.GOV)

Provine, J., E-mail: jprovine@stanford.edu; Schindler, Peter; Kim, Yongmin

2016-06-15

The continued scaling in transistors and memory elements has necessitated the development of atomic layer deposition (ALD) of silicon nitride (SiN{sub x}), particularly for use a low k dielectric spacer. One of the key material properties needed for SiN{sub x} films is a low wet etch rate (WER) in hydrofluoric (HF) acid. In this work, we report on the evaluation of multiple precursors for plasma enhanced atomic layer deposition (PEALD) of SiN{sub x} and evaluate the film’s WER in 100:1 dilutions of HF in H{sub 2}O. The remote plasma capability available in PEALD, enabled controlling the density of the SiN{submore » x} film. Namely, prolonged plasma exposure made films denser which corresponded to lower WER in a systematic fashion. We determined that there is a strong correlation between WER and the density of the film that extends across multiple precursors, PEALD reactors, and a variety of process conditions. Limiting all steps in the deposition to a maximum temperature of 350 °C, it was shown to be possible to achieve a WER in PEALD SiN{sub x} of 6.1 Å/min, which is similar to WER of SiN{sub x} from LPCVD reactions at 850 °C.« less

Cobalt and iron segregation and nitride formation from nitrogen plasma treatment of CoFeB surfaces

NASA Astrophysics Data System (ADS)

Mattson, E. C.; Michalak, D. J.; Veyan, J. F.; Chabal, Y. J.

2017-02-01

Cobalt-iron-boron (CoFeB) thin films are the industry standard for ferromagnetic layers in magnetic tunnel junction devices and are closely related to the relevant surfaces of CoFe-based catalysts. Identifying and understanding the composition of their surfaces under relevant processing conditions is therefore critical. Here we report fundamental studies on the interaction of nitrogen plasma with CoFeB surfaces using infrared spectroscopy, x-ray photoemission spectroscopy, and low energy ion scattering. We find that, upon exposure to nitrogen plasma, clean CoFeB surfaces spontaneously reorganize to form an overlayer comprised of Fe2N3 and BN, with the Co atoms moved well below the surface through a chemically driven process. Subsequent annealing to 400 °C removes nitrogen, resulting in a Fe-rich termination of the surface region.

Modeling the Gas Nitriding Process of Low Alloy Steels

NASA Astrophysics Data System (ADS)

Yang, M.; Zimmerman, C.; Donahue, D.; Sisson, R. D.

2013-07-01

The effort to simulate the nitriding process has been ongoing for the last 20 years. Most of the work has been done to simulate the nitriding process of pure iron. In the present work a series of experiments have been done to understand the effects of the nitriding process parameters such as the nitriding potential, temperature, and time as well as surface condition on the gas nitriding process for the steels. The compound layer growth model has been developed to simulate the nitriding process of AISI 4140 steel. In this paper the fundamentals of the model are presented and discussed including the kinetics of compound layer growth and the determination of the nitrogen diffusivity in the diffusion zone. The excellent agreements have been achieved for both as-washed and pre-oxided nitrided AISI 4140 between the experimental data and simulation results. The nitrogen diffusivity in the diffusion zone is determined to be constant and only depends on the nitriding temperature, which is ~5 × 10-9 cm2/s at 548 °C. It proves the concept of utilizing the compound layer growth model in other steels. The nitriding process of various steels can thus be modeled and predicted in the future.

Low-temperature ({<=}200 Degree-Sign C) plasma enhanced atomic layer deposition of dense titanium nitride thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samal, Nigamananda; Du Hui; Luberoff, Russell

Titanium nitride (TiN) has been widely used in the semiconductor industry for its diffusion barrier and seed layer properties. However, it has seen limited adoption in other industries in which low temperature (<200 Degree-Sign C) deposition is a requirement. Examples of applications which require low temperature deposition are seed layers for magnetic materials in the data storage (DS) industry and seed and diffusion barrier layers for through-silicon-vias (TSV) in the MEMS industry. This paper describes a low temperature TiN process with appropriate electrical, chemical, and structural properties based on plasma enhanced atomic layer deposition method that is suitable for themore » DS and MEMS industries. It uses tetrakis-(dimethylamino)-titanium as an organometallic precursor and hydrogen (H{sub 2}) as co-reactant. This process was developed in a Veeco NEXUS Trade-Mark-Sign chemical vapor deposition tool. The tool uses a substrate rf-biased configuration with a grounded gas shower head. In this paper, the complimentary and self-limiting character of this process is demonstrated. The effects of key processing parameters including temperature, pulse time, and plasma power are investigated in terms of growth rate, stress, crystal morphology, chemical, electrical, and optical properties. Stoichiometric thin films with growth rates of 0.4-0.5 A/cycle were achieved. Low electrical resistivity (<300 {mu}{Omega} cm), high mass density (>4 g/cm{sup 3}), low stress (<250 MPa), and >85% step coverage for aspect ratio of 10:1 were realized. Wet chemical etch data show robust chemical stability of the film. The properties of the film have been optimized to satisfy industrial viability as a Ruthenium (Ru) preseed liner in potential data storage and TSV applications.« less

Deposition of silicon nitride from SiCl4 and NH3 in a low pressure RF plasma

NASA Technical Reports Server (NTRS)

Ron, Y.; Raveh, A.; Carmi, U.; Inspektor, A.; Avni, R.

1983-01-01

Silicon nitride coatings were deposited in a low-pressure (1-10 Torr) RF plasma from SiCl4 and NH3 in the presence of argon onto stainless martensitic steel grounded and floating substrates at 300 C and 440 C respectively. The heating of the substrates depends mainly on the position and the induced RF power. The coatings were identified as silicon nitride by X-ray investigation and were found to contain chlorine by energy-dispersive analysis of X-rays. The growth rate, the microhardness and the chlorine concentration of the coatings were determined as a function of the total gas pressure, the RF power input and the NH3-to-SiCl4 ratio. It was observed that the coatings on the floating substrates have higher deposition rates and are of superior quality.

Optimization Study of Pulsed DC Nitrogen-Hydrogen Plasma in the Presence of an Active Screen Cage

NASA Astrophysics Data System (ADS)

Saeed, A.; W. Khan, A.; F., Jan; U. Shah, H.; Abrar, M.; Zaka-Ul-Islam, M.; Khalid, M.; Zakaullah, M.

2014-05-01

A glow discharge plasma nitriding reactor in the presence of an active screen cage is optimized in terms of current density, filling pressure and hydrogen concentrations using optical emission spectroscopy (OES). The samples of AISI 304 are nitrided for different treatment times under optimum conditions. The treated samples were analyzed by X-ray diffraction (XRD) to explore the changes induced in the crystallographic structure. The XRD pattern confirmed the formation of iron and chromium nitrides arising from incorporation of nitrogen as an interstitial solid solution in the iron lattice. A Vickers microhardness tester was used to evaluate the surface hardness as a function of treatment time (h). The results showed clear evidence of improved surface hardness and a substantial amount of decrease in the treatment time compared with the previous work.

Thermal conversion of an iron nitride-silicon nitride precursor into a ferromagnetic nanocomposite

NASA Astrophysics Data System (ADS)

Maya, L.; Thompson, J. R.; Song, K. J.; Warmack, R. J.

1998-01-01

Iron nitride films, FeN, in a pure form and in the form of a nanocomposite in silicon nitride were prepared by reactive sputtering using iron or iron disilicide, respectively, as targets in a nitrogen plasma. Iron nitride decomposes into the elements by heating in vacuum to 800 °C. Intermediate phases such as Fe2N or Fe4N form at lower temperatures. The nanocomposites contain the iron phases as particles with an average size of ˜5 nm dispersed in the amorphous silicon nitride matrix. The magnetic properties of the nanocomposites were established. The precursor FeN-Si3N4 film is paramagnetic, while the Fe-Si3N4, obtained by heating in vacuum, is ferromagnetic and shows typical superparamagnetic behavior. These films are of interest as recording media with superior chemical and mechanical stability and may be encoded by localized heating.

Transmission of Free Radicals through and Damage to Freestanding Single and Multilayer Dielectric Film

NASA Astrophysics Data System (ADS)

Choudhury, Faraz Anwar

A high concentration of free radicals is present in many processing plasmas, which affects the processing conditions and the properties of materials exposed to the plasma. Measuring the types and concentrations of free radicals present in the plasma is critical in order to determine their effects on the materials being processed. Current methods for detecting free radicals in a plasma require multiple expensive and bulky instruments, complex setups and often modifications to the plasma reactor. In this work, we present a simple technique that detects reactive-oxygen radicals incident on a surface from a plasma. The measurements are made using a fluorophore dye that is commonly used in biological and cellular systems for assay labeling in liquids. Using fluorometric analysis, it was found that the fluorophore reacts with oxygen radicals incident from the plasma, which is indicated by degradation of its fluorescence. As plasma power was increased, the quenching of the fluorescence significantly increased. Both immobilized and non-immobilized fluorophore dyes were used and the results indicate that both states function effectively under vacuum conditions. Using radical-sensitive dyes and free-standing films, the transmission of oxygen radicals through silicon nitride and silicon dioxide dielectric films is measured and their absorption lengths are determined. The absorption lengths were found to be 33, 37 and 40 nm for 15, 30 and 45-minute oxygen plasma exposures respectively. FTIR and XRR measurements show that a silicon oxynitride-like layer forms on the surface of the film which has a lower density than silicon nitride. The increase in absorption length with plasma-exposure time is attributed to the formation of the surface layer. In silicon dioxide films, the absorption length of oxygen radicals was found to be 70 nm after 20 minutes of plasma exposure. After 30 minutes of plasma exposure under the same conditions, the absorption length was reduced to 66 nm. XRR and FTIR measurements both reveal that the oxygen plasma exposure leads to surface oxidation of the silicon dioxide film and the formation of a denser surface layer which restricts the transmission of the radicals through the film. It was found that the extent of modification of the film partially depends on the radical dose. The calculated enthalpies of the reactions show that they are all exothermic reactions, however, the radicals need enough energy to overcome the activation energy for the reaction to take place.

Nitride microlens arrays for blue and ultraviolet wavelength applications

NASA Astrophysics Data System (ADS)

Oder, T. N.; Shakya, J.; Lin, J. Y.; Jiang, H. X.

2003-05-01

Nitride microlens arrays with sizes as small as 10 μm in diameter have been fabricated on GaN and AlN epilayers using the method of photoresist reflow and inductively coupled plasma dry etching. The focal lengths of the microlenses varied from 7-30 μm as determined by theoretical fitting as well as by the near-field scanning optical microscopy measurement. Scanning electron and atomic force microscopies were used to obtain the surface profile of the microlenses which were found to match very well with hemispherical fitting and a surface roughness value around 1 nm was obtained. Nitride microlens arrays would be naturally chosen for green/blue to deep ultraviolet wavelength applications. In addition, nitride microlenses offer the possibility of integrating nitride-based microsize photonic devices as well as of coupling light into, out of, and between arrays of III-nitride emitters for other applications, such as spatially resolved fluorescence spectroscopy studies of biological and medical systems and optical links, thereby further expanding the applications of III nitrides.

Process for the production of metal nitride sintered bodies and resultant silicon nitride and aluminum nitride sintered bodies

NASA Technical Reports Server (NTRS)

Yajima, S.; Omori, M.; Hayashi, J.; Kayano, H.; Hamano, M.

1983-01-01

A process for the manufacture of metal nitride sintered bodies, in particular, a process in which a mixture of metal nitrite powders is shaped and heated together with a binding agent is described. Of the metal nitrides Si3N4 and AIN were used especially frequently because of their excellent properties at high temperatures. The goal is to produce a process for metal nitride sintered bodies with high strength, high corrosion resistance, thermal shock resistance, thermal shock resistance, and avoidance of previously known faults.

Recent progress in plasma-assisted synthesis and modification of 2D materials

NASA Astrophysics Data System (ADS)

Han, Zhao Jun; Murdock, Adrian T.; Seo, Dong Han; Bendavid, Avi

2018-07-01

Plasma represents an important technique for both the synthesis and modification of two-dimensional (2D) materials, owing to the unique plasma-material interactions which can enable effective energy transfer at the nanoscale. Non-equilibrium and non-thermal plasma techniques have been widely applied on various 2D materials, including graphene, silicene, germanene, phosphorene, hexagonal boron nitride (h-BN), and transition metal dichalcogenides such as MoS2 and WS2. Here, we review the recent progress in plasma-assisted synthesis and modification (e.g. functionalisation, doping and etching) of 2D materials and discuss the potential applications of this unique branch of 2D materials. Challenges and future research opportunities in the relevant research field are also discussed. The primary aim of this Review is to provide a better understanding of the plasma-assisted processes and to promote the utilization of 2D materials for advanced electronic, optoelectronic, sensing and energy storage applications.

Viscoelastic Behavior of PDMS Filled with Boron Nitrides

NASA Astrophysics Data System (ADS)

Bian, J. F.; Weinkauf, D. H.; Jeon, H. S.

2004-03-01

The addition of high thermal conductive filler particles such as boron nitride, aluminum nitride, or carbon fiber is an effective way to increase the thermal conductivity of polymeric materials for the industrial applications such as electronic packaging materials, encapsulants, and thermal fluids among others. The effects of particle dispersions, concentrations, and the interactions between BN and polymer matrix on the viscoelastic properties of the boron nitride (BN)/polydimethylsiloxane (PDMS) composites prepared by mechanical mixing are investigated using oscillatory shear rheology. Both untreated and plasma treated boron nitride (BNP) particles with hexafluoropropylene oxide monomers have been used in this study. The addition of the plasma treated BN particles to the PDMS matrix decrease significantly the complex viscosity as well as storage and loss modulus of the composites due to the reduced interfacial energy between the surface of BNP and PDMS chains. For the PDMS/BN and PDMS/BNP composites, the maximum volume packing fraction ( ˜0.4) of the particles has been determined from the complex viscosity as a function of the frequency. Additionally, the shear-induced alignment of the BN particles dispersed in the PDMS matrix decreases the viscoelastic properties of the composites with the irregular oscillations which is related to the network formation of dispersed BN particles at the higher volume fractions (> ˜0.2).

Effect of laser power on the microstructure and mechanical properties of TiN/Ti3Al composite coatings on Ti6Al4V

NASA Astrophysics Data System (ADS)

Liu, Zhengdao; Zhang, Xiancheng; Xuan, Fuzhen; Wang, Zhengdong; Tu, Shandong

2013-07-01

Laser nitriding is one of the effective techniques to improve the surface properties of titanium alloys and has potential application in the life extension of last-stage steam turbine blades. However, cracking of surface coating is a common problem due to heat concentration in laser nitriding process. Conventionally, the cracks can be avoided through heat treatment, which may have an important influence on the mechanical properties of coating. Crack-free TiN/Ti3Al IMC coatings on Ti6Al4V are prepared by plasma spraying and laser nitriding. The microstructures, phase constitutes and compositions of the coating are observed and analyzed with scanning electron microscopy(SEM), X-ray diffraction(XRD) and X-ray energy-dispersive spectroscopy(EDS). Microhardness, elastic modulus, fracture toughness of the coating are measured. The results show that the crack- and pore-free IMC coatings can be made through the proposed method; with increasing laser power, the amount and density of TiN phase in the coating first increased and then decreased, leading to the similar trend of microhardness and elastic modulus and the reverse trend of fracture toughness of the coating. Both the average microhardness and elastic modulus of the coating increase three times higher than those of the substrate. The volume fraction of the TiN reinforced phase in composite can be controlled by varying the laser power and the cracking problem in laser nitriding process is successfully solved.

Method of chemical vapor deposition of boron nitride using polymeric cyanoborane

DOEpatents

Maya, L.

1994-06-14

Polymeric cyanoborane is volatilized, decomposed by thermal or microwave plasma energy, and deposited on a substrate as an amorphous film containing boron, nitrogen and carbon. Residual carbon present in the film is removed by ammonia treatment at an increased temperature, producing an adherent, essentially stoichiometric boron nitride film. 11 figs.

Radio Frequency Plasma Synthesis of Boron Nitride Nanotubes (BNNTs) for Structural Applications. Part II

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Alexa, Joel A.; Jensen, Brian J.

2016-01-01

Boron nitride nanotubes (BNNTs) are more thermally and chemically compatible with metal- and ceramic-matrix composites than carbon nanotubes (CNTs). The lack of an abundant supply of defect-free, high-aspect-ratio BNNTs has hindered development as reinforcing agents in structural materials. Recent activities at the National Research Council - Canada (NRC-C) and the University of California - Berkeley (UC-B) have resulted in bulk synthesis of few-walled, small diameter BNNTs. Both processes employ induction plasma technology to create boron vapor and highly reactive nitrogen species at temperatures in excess of 8000 K. Subsequent recombination under controlled cooling conditions results in the formation of BNNTs at a rate of 20 g/hr and 35 g/hr, respectively. The end product tends to consist of tangled masses of fibril-, sheet-, and cotton candy-like materials, which accumulate within the processing equipment. The radio frequency plasma spray (RFPS) facility at NASA Langley (LaRC), developed for metallic materials deposition, has been re-tooled for in-situ synthesis of BNNTs. The NRC-C and UC-B facilities comprise a 60 kW RF torch, a reactor with a stove pipe geometry, and a filtration system. In contrast, the LaRC facility has a 100 kW torch mounted atop an expansive reaction chamber coupled with a cyclone separator. The intent is to take advantage of both the extra power and the equipment configuration to simultaneously produce and gather BNNTs in a macroscopic form amenable to structural material applications.

Temporally and spatially resolved plasma spectroscopy in pulsed laser deposition of ultra-thin boron nitride films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Glavin, Nicholas R., E-mail: nicholas.glavin.1@us.af.mil, E-mail: andrey.voevodin@us.af.mil; School of Mechanical Engineering and Birck Nanotechnology Center, Purdue University, West Lafayette, Indiana 47907; Muratore, Christopher

2015-04-28

Physical vapor deposition (PVD) has recently been investigated as a viable, alternative growth technique for two-dimensional materials with multiple benefits over other vapor deposition synthesis methods. The high kinetic energies and chemical reactivities of the condensing species formed from PVD processes can facilitate growth over large areas and at reduced substrate temperatures. In this study, chemistry, kinetic energies, time of flight data, and spatial distributions within a PVD plasma plume ablated from a boron nitride (BN) target by a KrF laser at different pressures of nitrogen gas were investigated. Time resolved spectroscopy and wavelength specific imaging were used to identifymore » and track atomic neutral and ionized species including B{sup +}, B*, N{sup +}, N*, and molecular species including N{sub 2}*, N{sub 2}{sup +}, and BN. Formation and decay of these species formed both from ablation of the target and from interactions with the background gas were investigated and provided insights into fundamental growth mechanisms of continuous, amorphous boron nitride thin films. The correlation of the plasma diagnostic results with film chemical composition and thickness uniformity studies helped to identify that a predominant mechanism for BN film formation is condensation surface recombination of boron ions and neutral atomic nitrogen species. These species arrive nearly simultaneously to the substrate location, and BN formation occurs microseconds before arrival of majority of N{sup +} ions generated by plume collisions with background molecular nitrogen. The energetic nature and extended dwelling time of incident N{sup +} ions at the substrate location was found to negatively impact resulting BN film stoichiometry and thickness. Growth of stoichiometric films was optimized at enriched concentrations of ionized boron and neutral atomic nitrogen in plasma near the condensation surface, providing few nanometer thick films with 1:1 BN stoichiometry and good thicknesses uniformity over macroscopic areas.« less

The effect of processing conditions on the GaAs/plasma-grown insulator interface

NASA Technical Reports Server (NTRS)

Hshieh, F. I.; Borrego, J. M.; Ghandhi, S. K.

1986-01-01

The effect of processing conditions on the interface state density was evaluated from C-V measurements on metal-oxide-semiconductor capacitors. The optimum processing conditions for the minimum surface state density was found to be related to the postoxidation annealing temperature and time, and was independent of chemical treatments prior to oxidation. Annealing at the optimum condition (i.e., at 350 C for 1 h in either nitrogen or hydrogen gas, with or without an aluminum pattern on the oxide) reduces the fast surface state density by about one order of magnitude. By using a nitrogen/oxygen plasma, the static dielectric constant of the oxide decreased as the N/O ratio was increased, and nitrogen was incorporated into the oxide. In addition, the fast surface state density was reduced as a result of this nitridation process.

Nitriding of titanium by NH{sub 3} RF plasma: a study of the corrosion resistance and the mechanical properties of the protective films formed at the solid surface

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bellakhal, N

2002-12-01

The exposure of a titanium sample to an NH{sub 3} low pressure plasma leads to the formation of a nitriding layer. The products formed at the titanium surface were identified by XRD spectroscopy. The modification of the corrosion resistance characteristics of titanium due to the NH{sub 3} plasma treatment were investigated by electrochemical tests. The recorded polarization curves of the treated titanium samples were used to determine the values of the corrosion potential E{sub corr}. This study confirms the increasing of the corrosion resistance as a function of the time exposure and the injected electric power in the silica reactor.more » The plasma treatment also induces drastic changes of the titanium target in hardness.« less

Preparation and study of Titanium Nitride films by reactive sputtering and an investigation of target poisoning during the process

NASA Astrophysics Data System (ADS)

Aziz, Tareque; Rumaiz, Abdul

Titanium Nitride (TiNx) thin films were prepared by reactive dc sputtering in presence of Ar-N2 plasma. The thin films were grown on Quartz and pure Si surfaces. The Ar-N2 content ratio was gradually varied while the substrate and the Titanium target were kept at room temperature. Structural properties, optical and electrical properties of the thin films were studied by using X-ray Photoelectron Spectroscopy (XPS) and XRD and 4 probe resistivity measurement. Target poisoning of the Ti target was also studied by varying reactive gas concentration and measuring the target current. A study of target current vs growth rate of the films was performed to investigate the onset of ``poison'' mode.Although there was an insignificant drop in plasma current, we noticed a drop in the deposition rate. This result was tested against Monte Carlo simulations using SRIM simulations. Effects of annealing on the crystallinity and the sheet resistance will also be discussed. The work has been supported by BSA,DOE.

A novel technique based on a plasma focus device for nano-porous gallium nitride formation on P-type silicon

NASA Astrophysics Data System (ADS)

Sharifi Malvajerdi, S.; Salar Elahi, A.; Habibi, M.

2017-04-01

A new deposition formation was observed with a Mather-type Plasma Focus Device (MPFD). MPFD was unitized to fabricate porous Gallium Nitride (GaN) on p-type Silicon (Si) substrate with a (100) crystal orientation for the first time in a deposition process. GaN was deposited on Si with 4 and 7 shots. The samples were subjected to a 3 phase annealing procedure. First, the semiconductors were annealed in the PFD with nitrogen plasma shots after their deposition. Second, a thermal chemical vapor deposition annealed the samples for 1 h at 1050 °C by nitrogen gas at a pressure of 1 Pa. Finally, an electric furnace annealed the samples for 1 h at 1150 °C with continuous flow of nitrogen. Porous GaN structures were observed by Field emission scanning electron microscopy and atomic force microscopy. Furthermore, X-Ray diffraction analysis was carried out to determine the crystallinity of GaN after the samples were annealed. Energy-Dispersive X-Ray Spectroscopy indicated the amount of gallium, nitrogen, and oxygen due to the self-oxidation of the samples. Photoluminescence spectroscopy revealed emissions at 2.94 eV and 3.39 eV, which shows that hexagonal wurtzite crystal structures were formed.

Atomic-scale etching of hexagonal boron nitride for device integration based on two-dimensional materials.

PubMed

Park, Hamin; Shin, Gwang Hyuk; Lee, Khang June; Choi, Sung-Yool

2018-05-29

Hexagonal boron nitride (h-BN) is considered an ideal template for electronics based on two-dimensional (2D) materials, owing to its unique properties as a dielectric film. Most studies involving h-BN and its application to electronics have focused on its synthesis using techniques such as chemical vapor deposition, the electrical analysis of its surface state, and the evaluation of its performance. Meanwhile, processing techniques including etching methods have not been widely studied despite their necessity for device fabrication processes. In this study, we propose the atomic-scale etching of h-BN for integration into devices based on 2D materials, using Ar plasma at room temperature. A controllable etching rate, less than 1 nm min-1, was achieved and the low reactivity of the Ar plasma enabled the atomic-scale etching of h-BN down to a monolayer in this top-down approach. Based on the h-BN etching technique for achieving electrical contact with the underlying molybdenum disulfide (MoS2) layer of an h-BN/MoS2 heterostructure, a top-gate MoS2 field-effect transistor (FET) with h-BN gate dielectric was fabricated and characterized by high electrical performance based on the on/off current ratio and carrier mobility.

Making AlN(x) Tunnel Barriers Using a Low-Energy Nitrogen-Ion Beam

NASA Technical Reports Server (NTRS)

Kaul, Anupama; Kleinsasser, Alan; Bumble, Bruce; LeDuc, Henry; Lee, Karen

2005-01-01

A technique based on accelerating positive nitrogen ions onto an aluminum layer has been demonstrated to be effective in forming thin (<2 nm thick) layers of aluminum nitride (AlN(x)) for use as tunnel barriers in Nb/Al-AlN(x)/Nb superconductor/insulator/ superconductor (SIS) Josephson junctions. AlN(x) is the present material of choice for tunnel barriers because, to a degree greater than that of any other suitable material, it offers the required combination of low leakage current at high current density and greater thermal stability. While ultra-thin AlN films with good thickness and stoichiometry control are easily formed using techniques such as reactive molecular beam epitaxy and chemical vapor deposition, growth temperatures of 900 C are necessary for the dissociative adsorption of nitrogen from either nitrogen (N2) or ammonia (NH3). These growth temperatures are prohibitively high for the formation of tunnel barriers on Nb films because interfacial reactions at temperatures as low as 200 to 300 C degrade device properties. Heretofore, deposition by reactive sputtering and nitridation of thin Al layers with DC and RF nitrogen plasmas have been successfully used to form AlN barriers in SIS junctions. However, precise control over critical current density Jc has proven to be a challenge, as is attaining adequate process reproducibility from system to system. The present ion-beam technique is an alternative to the plasma or reactive sputtering techniques as it provides a highly controlled arrival of reactive species, independent of the electrical conditions of the substrate or vacuum chamber. Independent and accurate control of parameters such as ion energy, flux, species, and direction promises more precise control of film characteristics such as stoichiometry and thickness than is the case with typical plasma processes. In particular, the background pressure during ion-beam nitride growth is 2 or 3 orders of magnitude lower, minimizing the formation of compounds with contaminants, which is critical in devices the performance of which is dictated by interfacial characteristics. In addition, the flux of incoming species can be measured in situ using ion probes so that the dose can be controlled accurately. The apparatus used in the present ion-beam technique includes a vacuum chamber containing a commercial collimated- ion-beam source, a supply of nitrogen and argon, and an ion probe for measuring the ion dose. Either argon or nitrogen can be used as the feed gases for the ion source, depending on whether cleaning of the substrate or growth of the nitride, respectively, is desired. Once the Nb base electrode and Al proximity layer have been deposited, the N2 gas line to the ion beam is vented and purged, and the ion-source is turned on until a stable discharge is obtained. The substrate is moved over the ion-beam source to expose the Al surface layer to the ion beam (see figure) for a specified duration for the formation of the nitride tunnel barrier. Next, the Nb counter-electrode layer is deposited on the nitride surface layer. The Nb/Al- AlN(x)/Nb-trilayer-covered substrate is then patterned into individual devices by use of conventional integrated-circuit processing techniques.

Boron nitride microfibers grown by plasma-assisted laser chemical vapor deposition without a metal catalyst

NASA Astrophysics Data System (ADS)

Komatsu, Shojiro; Kazami, Daisuke; Tanaka, Hironori; Shimizu, Yoshiki; Moriyoshi, Yusuke; Shiratani, Masaharu; Okada, Katsuyuki

2006-04-01

Boron nitride fibers were found to grow on polycrystalline nickel and Si (100) substrates by plasma-assisted laser chemical vapor deposition from B2H6+NH3 using an excimer laser at 193nm. Their diameter was typically a few hundreds of nanometers, while the length was a few tens of micrometers. They were stoichiometric or boron-rich BN in chemical composition. When the substrate was rotated during deposition, spiral fibers were found to grow. We conclude that they grew with the help of laser light by other than the vapor - liquid - solid mechanism.

Plasma-Enhanced Pulsed Laser Deposition of Wide Bandgap Nitrides for Space Power Applications

NASA Technical Reports Server (NTRS)

Triplett, G. E., Jr.; Durbin, S. M.

2004-01-01

The need for a reliable, inexpensive technology for small-scale space power applications where photovoltaic or chemical battery approaches are not feasible has prompted renewed interest in radioisotope-based energy conversion devices. Although a number of devices have been developed using a variety of semiconductors, the single most limiting factor remains the overall lifetime of the radioisotope battery. Recent advances in growth techniques for ultra-wide bandgap III-nitride semiconductors provide the means to explore a new group of materials with the promise of significant radiation resistance. Additional benefits resulting from the use of ultra-wide bandgap materials include a reduction in leakage current and higher operating voltage without a loss of energy transfer efficiency. This paper describes the development of a novel plasma-enhanced pulsed laser deposition system for the growth of cubic boron nitride semiconducting thin films, which will be used to construct pn junction devices for alphavoltaic applications.

Caracterisation of Titanium Nitride Layers Deposited by Reactive Plasma Spraying

NASA Astrophysics Data System (ADS)

Roşu, Radu Alexandru; Şerban, Viorel-Aurel; Bucur, Alexandra Ioana; Popescu, Mihaela; Uţu, Dragoş

2011-01-01

Forming and cutting tools are subjected to the intense wear solicitations. Usually, they are either subject to superficial heat treatments or are covered with various materials with high mechanical properties. In recent years, thermal spraying is used increasingly in engineering area because of the large range of materials that can be used for the coatings. Titanium nitride is a ceramic material with high hardness which is used to cover the cutting tools increasing their lifetime. The paper presents the results obtained after deposition of titanium nitride layers by reactive plasma spraying (RPS). As deposition material was used titanium powder and as substratum was used titanium alloy (Ti6Al4V). Macroscopic and microscopic (scanning electron microscopy) images of the deposited layers and the X ray diffraction of the coatings are presented. Demonstration program with layers deposited with thickness between 68,5 and 81,4 μm has been achieved and presented.

Surface passivation of InGaP/GaAs HBT using silicon-nitride film deposited by ECR CVD plasma

NASA Astrophysics Data System (ADS)

Manera, L. T.; Zoccal, L. B.; Diniz, J. A.; Tatsch, P. J.; Doi, I.

2008-07-01

In this paper we have developed a passivation technique with silicon-nitride (SiN X) film that requires no surface pre-treatment, and is fully compatible to monolithic microwave integrated circuits (MMICs). The nitride depositions were carried out by ECR-CVD (electron cyclotron resonance-chemical vapor deposition) directly over InGaP/GaAs heterojunction structures, which are used for heterojunction bipolar transistors (HBTs). Optical emission spectrometry (OES) was used for plasma characterization, and low formation of H and NH molecules in the gas phase was detected at pressure of 2.5 mTorr. These molecules can degrade III-V semiconductor surfaces due to the preferential loss of As or P and hydrogen incorporation at the substrate. The substrates were cleaned with organic solvents using a Sox-let distillate. The ECR depositions were carried out at a fixed substrate temperature of 20 °C, SiH 4/N 2 flow ratio of 1, Ar flow of 5 sccm pressure of 2.5 mTorr and microwave (2.45 GHz) power of 250 W and RF (13.56 MHz) power of 4 W. We have applied this film for InGaP/GaAs HBT fabrication process with excellent results, where two major contribuiton is related to this passivation technique, the enhancement in the transistor dc gain β and the improvement in the signal-to-noise ratio when compared unpassivated and passivated devices.

Surface reconstruction of GaAs(001) nitrided under the controlled As partial pressure [rapid communication

NASA Astrophysics Data System (ADS)

Imayoshi, Takahiro; Oigawa, Haruhiro; Shigekawa, Hidemi; Tokumoto, Hiroshi

2003-08-01

Under the controlled As partial pressure, the nitridation process of GaAs(0 0 1)-(2 × 4) surface was studied using a scanning tunneling microscope (STM) combined with an electron cyclotron resonance plasma-assisted molecular beam epitaxy system. With either prolonging the nitridation time or decreasing the As partial pressure, the previously reported (3 × 3) structure with two dimers per surface cell ((3 × 3)-2D) was found to progressively convert into a new (3 × 3) structure characterized by one dimer per surface cell ((3 × 3)-1D). Reversely the exposure to arsenic transformed the structure from (3 × 3)-1D to (3 × 3)-2D, suggesting that the topmost layer is composed of As 2-dimers. Based on these STM images together with the X-ray photoelectron spectroscopy data, we propose the new As 2-dimer coverage models to explain both (3 × 3)-1D and -2D structures involving the exchange reaction of arsenic with nitrogen in the subsurface region of GaAs.

Plasma synthesis and HPHT consolidation of BN nanoparticles, nanospheres, and nanotubes to produce nanocrystalline cubic boron nitride

NASA Astrophysics Data System (ADS)

Stout, Christopher

Plasma methods offer a variety of advantages to nanomaterials synthesis. The process is robust, allowing varying particle sizes and phases to be generated simply by modifying key parameters. The work here demonstrates a novel approach to nanopowder synthesis using inductively-coupled plasma to decompose precursor, which are then quenched to produce a variety of boron nitride (BN)-phase nanoparticles, including cubic phase, along with short-range-order nanospheres (e.g., nano-onions) and BN nanotubes. Cubic BN (c-BN) powders can be generated through direct deposition onto a chilled substrate. The extremely-high pyrolysis temperatures afforded by the equilibrium plasma offer a unique particle growth environment, accommodating long deposition times while exposing resulting powders to temperatures in excess of 5000K without any additional particle nucleation and growth. Such conditions can yield short-range ordered amorphous BN structures in the form of 20nm diameter nanospheres. Finally, when introducing a rapid-quenching counter-flow gas against the plasma jet, high aspect ratio nanotubes are synthesized, which are collected on substrate situated radially. The benefits of these morphologies are also evident in high-pressure/high-temperature consolidation experiments, where nanoparticle phases can offer a favorable conversion route to super-hard c-BN while maintaining nanocrystallinity. Experiments using these morphologies are shown to begin to yield c-BN conversion at conditions as low as 2.0 GPa and 1500°C when using micron sized c-BN seeding to create localized regions of high pressures due to Hertzian forces acting on the nanoparticles.

Plasma emission spectroscopy and its relation to the refractive index of silicon nitride thin films deposited by reactive magnetron sputtering

NASA Astrophysics Data System (ADS)

Sanginés, R.; Abundiz-Cisneros, N.; Hernández Utrera, O.; Diliegros-Godines, C.; Machorro-Mejía, R.

2018-03-01

In this work, we present a thorough study on the relation between the plasma emission and the change of the silicon nitride thin films refractive index. Thin films were grown by reactive magnetron direct current sputtering technique and deposited onto silicon wafers at different fluxes of Ar and N2 and at different working pressures. This procedure, at certain deposition parameters, produced poor quality films, i.e. films with refractive index other than pure Si3N4 films. The emission of the plasma was interrogated in real time by means of optical emission spectroscopy (OES) observing at the vicinity of the trget location. In addition, optical properties of the films were measured by in situ ellipsometric-spectroscopy and then correlated with OES observations. Changes in the film refractive index could be deduced from changes in plasma emission applying a principal component analysis.

Molecular Beam Epitaxial Growth of Iron Nitrides on Zinc-Blende Gallium Nitride(001)

NASA Astrophysics Data System (ADS)

Pak, Jeongihm; Lin, Wenzhi; Chinchore, Abhijit; Wang, Kangkang; Smith, Arthur R.

2008-03-01

Iron nitrides are attractive materials for their high magnetic moments, corrosion, and oxidation resistance. We present the successful epitaxial growth of iron nitride on zinc-blende gallium nitride (c-GaN) in order to develop a novel magnetic transition metal nitride/semiconductor system. First, GaN is grown on magnesium oxide (MgO) substrates having (001) orientation using rf N2-plasma molecular beam epitaxy. Then we grow FeN at substrate temperature of ˜ 210 ^oC up to a thickness of ˜ 10.5 nm. In-situ reflection high-energy electron diffraction (RHEED) is used to monitor the surface during growth. Initial results suggest that the epitaxial relationship is FeN[001] || GaN[001] and FeN[100] || GaN[100]. Work in progress is to investigate the surface using in-situ scanning tunneling microscopy (STM) to reveal the surface structure at atomic scale, as well as to explore more Fe-rich magnetic phases.

Tuning Material Properties of Oxides and Nitrides by Substrate Biasing during Plasma-Enhanced Atomic Layer Deposition on Planar and 3D Substrate Topographies

PubMed Central

2018-01-01

Oxide and nitride thin-films of Ti, Hf, and Si serve numerous applications owing to the diverse range of their material properties. It is therefore imperative to have proper control over these properties during materials processing. Ion-surface interactions during plasma processing techniques can influence the properties of a growing film. In this work, we investigated the effects of controlling ion characteristics (energy, dose) on the properties of the aforementioned materials during plasma-enhanced atomic layer deposition (PEALD) on planar and 3D substrate topographies. We used a 200 mm remote PEALD system equipped with substrate biasing to control the energy and dose of ions by varying the magnitude and duration of the applied bias, respectively, during plasma exposure. Implementing substrate biasing in these forms enhanced PEALD process capability by providing two additional parameters for tuning a wide range of material properties. Below the regimes of ion-induced degradation, enhancing ion energies with substrate biasing during PEALD increased the refractive index and mass density of TiOx and HfOx and enabled control over their crystalline properties. PEALD of these oxides with substrate biasing at 150 °C led to the formation of crystalline material at the low temperature, which would otherwise yield amorphous films for deposition without biasing. Enhanced ion energies drastically reduced the resistivity of conductive TiNx and HfNx films. Furthermore, biasing during PEALD enabled the residual stress of these materials to be altered from tensile to compressive. The properties of SiOx were slightly improved whereas those of SiNx were degraded as a function of substrate biasing. PEALD on 3D trench nanostructures with biasing induced differing film properties at different regions of the 3D substrate. On the basis of the results presented herein, prospects afforded by the implementation of this technique during PEALD, such as enabling new routes for topographically selective deposition on 3D substrates, are discussed. PMID:29554799

Deposition of magnesium nitride thin films on stainless steel-304 substrates by using a plasma focus device

NASA Astrophysics Data System (ADS)

Ramezani, Amir Hoshang; Habibi, Maryam; Ghoranneviss, Mahmood

2014-08-01

In this research, for the first time, we synthesize magnesium nitride thin films on 304-type stainless steel substrates using a Mather-type (2 kJ) plasma focus (PF) device. The films of magnesium nitride are coated with different number of focus shots (like 15, 25 and 35) at a distance of 8 cm from the anode tip and at 0° angular position with respect to the anode axis. For investigation of the structural properties and surface morphology of magnesium nitride films, we utilized the X-ray diffractometer (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) analysis, respectively. Also, the elemental composition is characterized by energy-dispersive X-ray (EDX) analysis. Furthermore, Vicker's microhardness is used to study the mechanical properties of the deposited films. The results show that the degree of crystallinity of deposited thin films (from XRD), the average size of particles and surface roughness (from AFM), crystalline growth of structures (from SEM) and the hardness values of the films depend on the number of focus shots. The EDX analysis demonstrates the existence of the elemental composition of magnesium in the deposited samples.

Atomic Layer Epitaxy of Aluminum Nitride: Unraveling the Connection between Hydrogen Plasma and Carbon Contamination.

PubMed

Erwin, Steven C; Lyons, John L

2018-06-13

Atomistic control over the growth of semiconductor thin films, such as aluminum nitride, is a long-sought goal in materials physics. One promising approach is plasma-assisted atomic layer epitaxy, in which separate reactant precursors are employed to grow the cation and anion layers in alternating deposition steps. The use of a plasma during the growth-most often a hydrogen plasma-is now routine and generally considered critical, but the precise role of the plasma is not well-understood. We propose a theoretical atomistic model and elucidate its consequences using analytical rate equations, density functional theory, and kinetic Monte Carlo statistical simulations. We show that using a plasma has two important consequences, one beneficial and one detrimental. The plasma produces atomic hydrogen in the gas phase, which is important for removing methyl radicals left over from the aluminum precursor molecules. However, atomic hydrogen also leads to atomic carbon on the surface and, moreover, opens a channel for trapping these carbon atoms as impurities in the subsurface region, where they remain as unwanted contaminants. Understanding this dual role leads us to propose a solution for the carbon contamination problem which leaves the main benefit of the plasma largely unaffected.

Functionalized boron nitride nanotubes

DOEpatents

Sainsbury, Toby; Ikuno, Takashi; Zettl, Alexander K

2014-04-22

A plasma treatment has been used to modify the surface of BNNTs. In one example, the surface of the BNNT has been modified using ammonia plasma to include amine functional groups. Amine functionalization allows BNNTs to be soluble in chloroform, which had not been possible previously. Further functionalization of amine-functionalized BNNTs with thiol-terminated organic molecules has also been demonstrated. Gold nanoparticles have been self-assembled at the surface of both amine- and thiol-functionalized boron nitride Nanotubes (BNNTs) in solution. This approach constitutes a basis for the preparation of highly functionalized BNNTs and for their utilization as nanoscale templates for assembly and integration with other nanoscale materials.

Role of Plasma Temperature and Residence Time in Stagnation Plasma Synthesis of c-BN Nanopowders

DTIC Science & Technology

2013-01-01

outer diameter of 15mm. A center injection 19 nozzle of 1.4mm diameter is implemented for precursor introduction. Plasma and sheath gas ... Gas Phase Synthesis of Nanoparticles..................................................... 5 2.2 Cubic Boron Nitride Synthesis...11 2.2.4 Effects of gas composition ............................................................................................ 11

Comparative study of ITO and TiN fabricated by low-temperature RF biased sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Simon, Daniel K., E-mail: daniel.simon@namlab.com; Schenk, Tony; Dirnstorfer, Ingo

2016-03-15

Radio frequency (RF) biasing induced by a second plasma source at the substrate is applied to low-temperature sputtering processes for indium tin oxide (ITO) and titanium nitride (TiN) thin films. Investigations on crystal structure and surface morphology show that RF-biased substrate plasma processes result in a changed growth regime with different grain sizes and orientations than those produced by processes without a substrate bias. The influence of the RF bias is shown comparatively for reactive RF-sputtered ITO and reactive direct-current-sputtered TiN. The ITO layers exhibit an improved electrical resistivity of 0.5 mΩ cm and an optical absorption coefficient of 0.5 × 10{sup 4 }cm{supmore » −1} without substrate heating. Room-temperature sputtered TiN layers are deposited that possess a resistivity (0.1 mΩ cm) of 3 orders of magnitude lower than, and a density (5.4 g/cm{sup 3}) up to 45% greater than, those obtained from layers grown using the standard process without a substrate plasma.« less

Enhancing the Hardness of Sintered SS 17-4PH Using Nitriding Process for Bracket Orthodontic Application

NASA Astrophysics Data System (ADS)

Suharno, B.; Supriadi, S.; Ayuningtyas, S. T.; Widjaya, T.; Baek, E. R.

2018-01-01

Brackets orthodontic create teeth movement by applying force from wire to bracket then transferred to teeth. However, emergence of friction between brackets and wires reduces load for teeth movement towards desired area. In order to overcome these problem, surface treatment like nitriding chosen as a process which could escalate efficiency of transferred force by improving material hardness since hard materials have low friction levels. This work investigated nitriding treatment to form nitride layer which affecting hardness of sintered SS 17-4PH. The nitride layers produced after nitriding process at various temperature i.e. 470°C, 500°C, 530°C with 8hr holding time under 50% NH3 atmosphere. Optical metallography was conducted to compare microstructure of base and surface metal while the increasing of surface hardness then observed using vickers microhardness tester. Hardened surface layer was obtained after gaseous nitriding process because of nitride layer that contains Fe4N, CrN and Fe-αN formed. Hardness layers can achieved value 1051 HV associated with varies thickness from 53 to 119 μm. The presence of a precipitation process occurring in conjunction with nitriding process can lead to a decrease in hardness due to nitrogen content diminishing in solid solution phase. This problem causes weakening of nitrogen expansion in martensite lattice.

Semiconductor/dielectric interface engineering and characterization

NASA Astrophysics Data System (ADS)

Lucero, Antonio T.

The focus of this dissertation is the application and characterization of several, novel interface passivation techniques for III-V semiconductors, and the development of an in-situ electrical characterization. Two different interface passivation techniques were evaluated. The first is interface nitridation using a nitrogen radical plasma source. The nitrogen radical plasma generator is a unique system which is capable of producing a large flux of N-radicals free of energetic ions. This was applied to Si and the surface was studied using x-ray photoelectron spectroscopy (XPS). Ultra-thin nitride layers could be formed from 200-400° C. Metal-oxide-semiconductor capacitors (MOSCAPs) were fabricated using this passivation technique. Interface nitridation was able to reduce leakage current and improve the equivalent oxide thickness of the devices. The second passivation technique studied is the atomic layer deposition (ALD) diethylzinc (DEZ)/water treatment of sulfur treated InGaAs and GaSb. On InGaAs this passivation technique is able to chemically reduce higher oxidation states on the surface, and the process results in the deposition of a ZnS/ZnO interface passivation layer, as determined by XPS. Capacitance-voltage (C-V) measurements of MOSCAPs made on p-InGaAs reveal a large reduction in accumulation dispersion and a reduction in the density of interfacial traps. The same technique was applied to GaSb and the process was studied in an in-situ half-cycle XPS experiment. DEZ/H2O is able to remove all Sb-S from the surface, forming a stable ZnS passivation layer. This passivation layer is resistant to further reoxidation during dielectric deposition. The final part of this dissertation is the design and construction of an ultra-high vacuum cluster tool for in-situ electrical characterization. The system consists of three deposition chambers coupled to an electrical probe station. With this setup, devices can be processed and subsequently electrically characterized without exposing the sample to air. This is the first time that such a system has been reported. A special air-gap C-V probe will allow top gated measurements to be made, allowing semiconductor-dielectric interfaces to be studied during device processing.

Silicon-on-Insulator Pin Diodes.

DTIC Science & Technology

1987-12-01

Thin (0.5 Micron) Silicon-on-Oxidized Silicon Fig. 2.8 SEM Photographs of CVD Silicon Dioxide on Aluminum 28 After 1500 0 C Anneal in Oxygen...silicon nitride over the silicon dioxide encapsu- -9- lation layer and by depositing the silicon dioxide with a plasma CVD process which uses N20 as...relief via thermal expansion matching varies lin- -27- A B Figure 2.8: SEM Photographs of CVD Silicon Dioxide on Aluminum after 15000 C Anneal in Oxygen

Gallium nitride nanoneedles grown in extremely non-equilibrium nitrogen plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mangla, O., E-mail: onkarmangla@gmail.com; Physics Department, Hindu College, University of Delhi, Delhi, 110007; Roy, S.

2016-05-23

In the present work, gallium nitride (GaN) nanoneedles are grown on quartz substrates using the high fluence ions of GaN produced by hot, dense and extremely non-equlibrium nitrogen plasma in a modified dense plasma focus device. The formation of nanoneedles is obtained from the scanning electron microscopy with mean size of the head of nanoneedles ~ 70 nm. The nanoneedles are found to be poly-crystalline when studied structurally through the X-ray diffraction. The optical properties of nanoneedles studied using absorption spectra which show more absorption for nanoneedles depsoited one shot of ions irradiation. In addition, the band gap of nanoneedles ismore » found to be increased as compared to bulk GaN. The obtained nanoneedles with increased band gap have potential applications in detector systems.« less

Tribological Properties of Surface-Textured and Plasma-Nitrided Pure Titanium Under Oil Lubrication Condition

NASA Astrophysics Data System (ADS)

Zhang, Baosen; Dong, Qiangsheng; Ba, Zhixin; Wang, Zhangzhong; Shi, Hancheng; Xue, Yanting

2018-01-01

Plasma nitriding was conducted as post-treatment for surface texture on pure titanium to obtain a continuous nitriding layer. Supersonic fine particles bombarding (SFPB) was carried out to prepare surface texture. The surface morphologies and chemical composition were analyzed using scanning electron microscope and energy disperse spectroscopy. The microstructures of modified layers were characterized by transmission electron microscope. The tribological properties of surface-textured and duplex-treated pure titanium under oil lubrication condition were systematically investigated in the ball-on-plate reciprocating mode. The effects of applied load and sliding velocity on the tribological behavior were analyzed. The results show that after duplex treatments, the grains size in modified layer becomes slightly larger, and hardness is obviously improved. Wear resistance of duplex-treated pure titanium is significantly improved referenced to untreated and surface-textured pure titanium, which is 3.22 times as much as untreated pure titanium and 2.15 times of that for surface-textured pure titanium, respectively.

Back scattering involving embedded silicon nitride (SiN) nanoparticles for c-Si solar cells

NASA Astrophysics Data System (ADS)

Ghosh, Hemanta; Mitra, Suchismita; Siddiqui, M. S.; Saxena, A. K.; Chaudhuri, Partha; Saha, Hiranmay; Banerjee, Chandan

2018-04-01

A novel material, structure and method of synthesis for dielectric light trapping have been presented in this paper. First, the light scattering behaviour of silicon nitride nanoparticles have been theoretically studied in order to find the optimized size for dielectric back scattering by FDTD simulations from Lumerical Inc. The optical results have been used in electrical analysis and thereby, estimate the effect of nanoparticles on efficiency of the solar cells depending on substrate thickness. Experimentally, silicon nitride (SiN) nanoparticles have been formed using hydrogen plasma treatment on SiN layer deposited by Plasma Enhanced Chemical Vapour Deposition (PECVD). The size and area coverage of the nanoparticles were controlled by varying the working pressure, power density and treatment duration. The nanoparticles were integrated with partial rear contact c-Si solar cells as dielectric back reflector structures for the light trapping in thin silicon solar cells. Experimental results revealed the increases of current density by 2.7% in presence of SiN nanoparticles.

Influences of urea and sodium nitrite on surface coating of plasma electrolytic oxidation

NASA Astrophysics Data System (ADS)

Yeh, Shang-Chun; Tsai, Dah-Shyang; Guan, Sheng-Yong; Chou, Chen-Chia

2015-11-01

Urea and sodium nitrite are generally viewed as nitridation additives in the electrolyte for plasma electrolytic oxidation (PEO) of aluminum alloys. We study the influences of these two convenient chemicals in presence of sodium aluminate and find very different effects on film growth. Urea addition enhances the nitrogen content of PEO layer, diminishes the layer thickness, increases the porosity, interferes with the α-alumina formation, and promotes precipitation in the electrolyte. Hence, the electrolytic urea content ought to be maintained less than 45 g dm-3. On the other hand, sodium nitrite behaves like an oxidation additive, more than a nitridation additive. NaNO2 addition effectively introduces nitrogen in the PEO layer at low concentration, yet the nitrogen content of oxide layer decreases with increasing NaNO2 concentration. The effects of NaNO2, such as increasing layer thickness, reducing porosity, promoting α-alumina formation are attributed to oxidation enhancement, not because of nitridation.

Detection of boron nitride radicals by emission spectroscopy in a laser-induced plasma

NASA Astrophysics Data System (ADS)

Dutouquet, C.; Acquaviva, S.; Hermann, J.

2001-06-01

Several vibrational bands of boron nitride radicals have been observed in a plasma produced by pulsed-laser ablation of a boron nitride target in low-pressure nitrogen or argon atmospheres. Using time- and space-resolved emission spectroscopic measurements with a high dynamic range, the most abundant isotopic species B 11N have been detected. The emission bands in the spectral range from 340 to 380 nm belong to the Δυ =-1, 0, +1 sequences of the triplet system (transition A 3Π-X 3Π). For positive identification, the molecular emission bands have been compared with synthetic spectra obtained by computer simulations. Furthermore, B 10N emission bands have been reproduced by computer simulation using molecular constants which have been deduced from the B 11N constants. Nevertheless, the presence of the lower abundant isotopic radical B 10N was not proved due the noise level which masked the low emission intensity of the B 10N band heads.

III-nitrides on oxygen- and zinc-face ZnO substrates

NASA Astrophysics Data System (ADS)

Namkoong, Gon; Burnham, Shawn; Lee, Kyoung-Keun; Trybus, Elaissa; Doolittle, W. Alan; Losurdo, Maria; Capezzuto, Pio; Bruno, Giovanni; Nemeth, Bill; Nause, Jeff

2005-10-01

The characteristics of III-nitrides grown on zinc- and oxygen-face ZnO by plasma-assisted molecular beam epitaxy were investigated. The reflection high-energy electron diffraction pattern indicates formation of a cubic phase at the interface between III-nitride and both Zn- and O-face ZnO. The polarity indicates that Zn-face ZnO leads to a single polarity, while O-face ZnO forms mixed polarity of III-nitrides. Furthermore, by using a vicinal ZnO substrate, the terrace-step growth of GaN was realized with a reduction by two orders of magnitude in the dislocation-related etch pit density to ˜108cm-2, while a dislocation density of ˜1010cm-2 was obtained on the on-axis ZnO substrates.

Tribological and microstructural characteristics of ion-nitrided steels

NASA Technical Reports Server (NTRS)

Spalvins, T.

1983-01-01

Three steels AISI 4140, AISI 4340 and AISI 304 stainless steel were ion nitrided in a plasma consisting of a 75:25 mixture of H2:N2, sometimes with a trace of CH4. Their surface topography was characterized by SEM and two distinct compound phases were identified: the gamma and the epsilon. The core-case hardness profiles were also established. The low Cr alloy steels have an extended diffusion zone in contrast to the 304 stainless steels which have a sharp interface. The depth of ion-nitriding is increased as the Cr content is decreased. Friction tests reveal that the gamma surface phase has a lower coefficient of friction than the epsilon phase. The lowest coefficient of friction is achieved when both the rider and the specimen surface are ion nitrided.

Microstructural Characteristics of Plasma Nitrided Layer on Hot-Rolled 304 Stainless Steel with a Small Amount of α-Ferrite

NASA Astrophysics Data System (ADS)

Xu, Xiaolei; Yu, Zhiwei; Cui, Liying; Niu, Xinjun; Cai, Tao

2016-02-01

The hot-rolled 304 stainless steel with γ-austenite and approximately 5 pct α-ferrite elongated along the rolling direction was plasma-nitrided at a low temperature of 693 K (420 °C). X-ray diffraction results revealed that the nitrided layer was mainly composed of the supersaturated solid solution of nitrogen in austenite ( γ N). Transmission electron microscopy (TEM) observations showed that the microstructure of the γ N phase exhibited "fracture factor contrast" reflective of the occurrence of fine pre-precipitations in γ N by the continuous precipitation. The occurrence of a diffuse scattering effect on the electron diffraction spots of γ N indicated that the pre-precipitation took place in γ N in the form of strongly bonded Cr-N clusters or pairs due to a strong attractive interaction of nitrogen with chromium. Scanning electron microscopy and TEM observations indicated that the discontinuous precipitation initiated from the γ/ α interfaces and grew from the austenite boundaries into austenite grains to form a lamellar structure consisting of CrN and ferrite. The orientation relationship between CrN and ferrite corresponded to a Baker-Nutting relationship: (100)CrN//(100) α ; [011]CrN//[001] α . A zigzag boundary line following the banded structure of alternating γ-austenite and elongated α-ferrite was presented between the nitrided layer and the substrate to form a continuous varying layer thickness, which resulted from the difference in diffusivities of nitrogen in α-ferrite and γ-austenite, along the γ/ α interfaces and through the lattice. Microstructural features similar to the γ N were also revealed in the ferrite of the nitrided layer by TEM. It was not excluded that a supersaturated solid solution of nitrogen in ferrite ( α N) formed in the nitrided layer.

Process for making transition metal nitride whiskers

DOEpatents

Bamberger, Carlos E.

1989-01-01

A process for making metal nitrides, particularly titanium nitride whiskers, using a cyanide salt as a reducing agent for a metal compound in the presence of an alkali metal oxide. Sodium cyanide, various titanates and titanium oxide mixed with sodium oxide react to provide titanium nitride whiskers that can be used as reinforcement to ceramic composites.

The automated array assembly task of the low-cost silicon solar array project, phase 2

NASA Technical Reports Server (NTRS)

Coleman, M. G.; Pryor, R. A.; Sparks, T. G.; Legge, R.; Saltzman, D. L.

1980-01-01

Several specific processing steps as part of a total process sequence for manufacturing silicon solar cells were studied. Ion implantation was identified as the preferred process step for impurity doping. Unanalyzed beam ion implantation was shown to have major cost advantages over analyzed beam implantation. Further, high quality cells were fabricated using a high current unanalyzed beam. Mechanically masked plasma patterning of silicon nitride was shown to be capable of forming fine lines on silicon surfaces with spacings between mask and substrate as great as 250 micrometers. Extensive work was performed on advances in plated metallization. The need for the thick electroless palladium layer was eliminated. Further, copper was successfully utilized as a conductor layer utilizing nickel as a barrier to copper diffusion into the silicon. Plasma etching of silicon for texturing and saw damage removal was shown technically feasible but not cost effective compared to wet chemical etching techniques.

Process dependency of radiation hardness of rapid thermal reoxidized nitrided gate oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weishin Lu; Kuanchin Lin; Jenngwo Hwu

The radiation hardness of MOS capacitors with various reoxidized nitrided oxide (RNO) structures is studied by changing the durations of rapid thermal processes during sample preparation and by applying irradiation-then-anneal (ITA) treatments on samples after preparation. It is found that the initial flatband voltage and midgap interface trap density of MOS capacitors exhibit turnaround'' dependency on the total time of nitridation and reoxidation processes. For samples with nitrided oxide (NO) structures, the radiation-induced variations of above parameters are also turnaround''-dependent on nitridation time. However, when the reoxidation process is performed, the radiation hardness for all samples will be gradually improvedmore » with increasing reoxidation time no matter what the nitridation time is. The most radiation-hard process for RNO structures is suggested. Finally, it is found that when ITA treatments are applied on samples after preparation, their radiation hardness is much improved.« less

Self-assembled growth of GaN nanowires on amorphous Al x O y : from nucleation to the formation of dense nanowire ensembles.

PubMed

Sobanska, M; Fernández-Garrido, S; Zytkiewicz, Z R; Tchutchulashvili, G; Gieraltowska, S; Brandt, O; Geelhaar, L

2016-08-12

We present a comprehensive description of the self-assembled nucleation and growth of GaN nanowires (NWs) by plasma-assisted molecular beam epitaxy on amorphous Al x O y buffers (a-Al x O y ) prepared by atomic layer deposition. The results are compared with those obtained on nitridated Si(111). Using line-of-sight quadrupole mass spectrometry, we analyze in situ the incorporation of Ga starting from the incubation and nucleation stages till the formation of the final nanowire ensemble and observe qualitatively the same time dependence for the two types of substrates. However, on a-Al x O y the incubation time is shorter and the nucleation faster than on nitridated Si. Moreover, on a-Al x O y we observe a novel effect of decrease in incorporated Ga flux for long growth durations which we explain by coalescence of NWs leading to reduction of the GaN surface area where Ga may reside. Dedicated samples are used to analyze the evolution of surface morphology. In particular, no GaN nuclei are detected when growth is interrupted during the incubation stage. Moreover, for a-Al x O y , the same shape transition from spherical cap-shaped GaN crystallites to the NW-like geometry is found as it is known for nitridated Si. However, while the critical radius for this transition is only slightly larger for a-Al x O y than for nitridated Si, the critical height is more than six times larger for a-Al x O y . Finally, we observe that in fully developed NW ensembles, the substrate no longer influences growth kinetics and the same N-limited axial growth rate is measured on both substrates. We conclude that the same nucleation and growth processes take place on a-Al x O y as on nitridated Si and that these processes are of a general nature. Quantitatively, nucleation proceeds somewhat differently, which indicates the influence of the substrate, but once shadowing limits growth processes to the upper part of the NW ensemble, they are not affected anymore by the type of substrate.

Initial evaluation and comparison of plasma damage to atomic layer carbon materials using conventional and low T{sub e} plasma sources

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jagtiani, Ashish V.; Miyazoe, Hiroyuki; Chang, Josephine

2016-01-15

The ability to achieve atomic layer precision is the utmost goal in the implementation of atomic layer etch technology. Carbon-based materials such as carbon nanotubes (CNTs) and graphene are single atomic layers of carbon with unique properties and, as such, represent the ultimate candidates to study the ability to process with atomic layer precision and assess impact of plasma damage to atomic layer materials. In this work, the authors use these materials to evaluate the atomic layer processing capabilities of electron beam generated plasmas. First, the authors evaluate damage to semiconducting CNTs when exposed to beam-generated plasmas and compare thesemore » results against the results using typical plasma used in semiconductor processing. The authors find that the beam generated plasma resulted in significantly lower current degradation in comparison to typical plasmas. Next, the authors evaluated the use of electron beam generated plasmas to process graphene-based devices by functionalizing graphene with fluorine, nitrogen, or oxygen to facilitate atomic layer deposition (ALD). The authors found that all adsorbed species resulted in successful ALD with varying impact on the transconductance of the graphene. Furthermore, the authors compare the ability of both beam generated plasma as well as a conventional low ion energy inductively coupled plasma (ICP) to remove silicon nitride (SiN) deposited on top of the graphene films. Our results indicate that, while both systems can remove SiN, an increase in the D/G ratio from 0.08 for unprocessed graphene to 0.22 to 0.26 for the beam generated plasma, while the ICP yielded values from 0.52 to 1.78. Generally, while some plasma-induced damage was seen for both plasma sources, a much wider process window as well as far less damage to CNTs and graphene was observed when using electron beam generated plasmas.« less

Optical and electrical characterization methods of plasma-induced damage in silicon nitride films

NASA Astrophysics Data System (ADS)

Kuyama, Tomohiro; Eriguchi, Koji

2018-06-01

We proposed evaluation methods of plasma-induced damage (PID) in silicon nitride (SiN) films. The formation of an oxide layer by air exposure was identified for damaged SiN films by X-ray photoelectron spectroscopy (XPS). Bruggeman’s effective medium approximation was employed for an optical model consisting of damaged and undamaged layers, which is applicable to an in-line monitoring by spectroscopic ellipsometry (SE). The optical thickness of the damaged layer — an oxidized layer — extended after plasma exposure, which was consistent with the results obtained by a diluted hydrofluoric acid (DHF) wet etching. The change in the conduction band edge of the damaged SiN films was presumed from two electrical techniques, i.e., current–voltage (I–V) measurement and time-dependent dielectric breakdown (TDDB) test with a constant voltage stress. The proposed techniques can be used for assigning the plasma-induced structural change in an SiN film widely used as an etch-protecting layer.

Structural, morphological and mechanical properties of niobium nitride thin films grown by ion and electron beams emanated from plasma

NASA Astrophysics Data System (ADS)

Siddiqui, Jamil; Hussain, Tousif; Ahmad, Riaz; Umar, Zeeshan A.; Abdus Samad, Ubair

2016-05-01

The influence of variation in plasma deposition parameters on the structural, morphological and mechanical characteristics of the niobium nitride films grown by plasma-emanated ion and electron beams are investigated. Crystallographic investigation made by X-ray diffractometer shows that the film synthesized at 10 cm axial distance with 15 plasma focus shots (PFS) exhibits better crystallinity when compared to the other deposition conditions. Morphological analysis made by scanning electron microscope reveals a definite granular pattern composed of homogeneously distributed nano-spheroids grown as clustered particles for the film synthesized at 10 cm axial distance for 15 PFS. Roughness analysis demonstrates higher rms roughness for the films synthesized at shorter axial distance and by greater number of PFS. Maximum niobium atomic percentage (35.8) and maximum average hardness (19.4 ± 0.4 GPa) characterized by energy-dispersive spectroscopy and nano-hardness analyzer respectively are observed for film synthesized at 10 cm axial distance with 15 PFS.

Selective dry etching of III-V nitrides in Cl{sub 2}/Ar, CH{sub 4}/H{sub 2}/Ar, ICi/Ar, and IBr/Ar

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vartuli, C.B.; Pearton, S.J.; MacKenzie, J.D.

1996-10-01

The selectivity for etching the binary (GaN, AlN, and InN) and ternary nitrides (InGaN and InAlN) relative to each other in Cl{sub 2}/Ar, CH{sub 4}/H{sub 2}/Ar, ICl/Ar, or IBr/Ar electron cyclotron resonance (ECR) plasmas, and Cl{sub 2}/Ar or CH{sub 4}/H{sub 2}/Ar reactive ion (RIE) plasmas was investigated. Cl-based etches appear to be the best choice for maximizing the selectivity of GaN over the other nitrides. GaN/AlN and GaN/InGaN etch rate ratios of {approximately} 10 were achieved at low RF power in Cl{sub 2}/Ar under ECR and RIE conditions, respectively. GaN/InN selectivity of 10 was found in ICl under ECR conditions.more » A relatively high selectivity (> 6) of InN/GaN was achieved in CH{sub 4}/H{sub 2}/Ar under ECR conditions at low RF powers (50 W). Since the high bond strengths of the nitrides require either high ion energies or densities to achieve practical etch rates it is difficult to achieve high selectivities.« less

Process for making transition metal nitride whiskers

DOEpatents

Bamberger, C.E.

1988-04-12

A process for making metal nitrides, particularly titanium nitride whiskers, using a cyanide salt as a reducing agent for a metal compound in the presence of an alkali metal oxide. Sodium cyanide, various titanates and titanium oxide mixed with sodium oxide react to provide titanium nitride whiskers that can be used as reinforcement to ceramic composites. 1 fig., 1 tab.

Nitride alloy layer formation of duplex stainless steel using nitriding process

NASA Astrophysics Data System (ADS)

Maleque, M. A.; Lailatul, P. H.; Fathaen, A. A.; Norinsan, K.; Haider, J.

2018-01-01

Duplex stainless steel (DSS) shows a good corrosion resistance as well as the mechanical properties. However, DSS performance decrease as it works under aggressive environment and at high temperature. At the mentioned environment, the DSS become susceptible to wear failure. Surface modification is the favourable technique to widen the application of duplex stainless steel and improve the wear resistance and its hardness properties. Therefore, the main aim of this work is to nitride alloy layer on the surface of duplex stainless steel by the nitriding process temperature of 400°C and 450°C at different time and ammonia composition using a horizontal tube furnace. The scanning electron microscopy and x-ray diffraction analyzer are used to analyse the morphology, composition and the nitrided alloy layer for treated DSS. The micro hardnesss Vickers tester was used to measure hardness on cross-sectional area of nitrided DSS. After nitriding, it was observed that the hardness performance increased until 1100 Hv0.5kgf compared to substrate material of 250 Hv0.5kgf. The thickness layer of nitride alloy also increased from 5μm until 100μm due to diffusion of nitrogen on the surface of DSS. The x-ray diffraction results showed that the nitride layer consists of iron nitride, expanded austenite and chromium nitride. It can be concluded that nitride alloy layer can be produced via nitriding process using tube furnace with significant improvement of microstructural and hardness properties.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Molecular carbon nitride ion beams for enhanced corrosion resistance of stainless steel

NASA Astrophysics Data System (ADS)

Markwitz, A.; Kennedy, J.

2017-10-01

A novel approach is presented for molecular carbon nitride beams to coat stainless surfaces steel using conventional safe feeder gases and electrically conductive sputter targets for surface engineering with ion implantation technology. GNS Science's Penning type ion sources take advantage of the breaking up of ion species in the plasma to assemble novel combinations of ion species. To test this phenomenon for carbon nitride, mixtures of gases and sputter targets were used to probe for CN+ ions for simultaneous implantation into stainless steel. Results from mass analysed ion beams show that CN+ and a variety of other ion species such as CNH+ can be produced successfully. Preliminary measurements show that the corrosion resistance of stainless steel surfaces increased sharply when implanting CN+ at 30 keV compared to reference samples, which is interesting from an application point of view in which improved corrosion resistance, surface engineering and short processing time of stainless steel is required. The results are also interesting for novel research in carbon-based mesoporous materials for energy storage applications and as electrode materials for electrochemical capacitors, because of their high surface area, electrical conductivity, chemical stability and low cost.

Moiré-Modulated Conductance of Hexagonal Boron Nitride Tunnel Barriers.

PubMed

Summerfield, Alex; Kozikov, Aleksey; Cheng, Tin S; Davies, Andrew; Cho, Yong-Jin; Khlobystov, Andrei N; Mellor, Christopher J; Foxon, C Thomas; Watanabe, Kenji; Taniguchi, Takashi; Eaves, Laurence; Novoselov, Kostya S; Novikov, Sergei V; Beton, Peter H

2018-06-27

Monolayer hexagonal boron nitride (hBN) tunnel barriers investigated using conductive atomic force microscopy reveal moiré patterns in the spatial maps of their tunnel conductance consistent with the formation of a moiré superlattice between the hBN and an underlying highly ordered pyrolytic graphite (HOPG) substrate. This variation is attributed to a periodc modulation of the local density of states and occurs for both exfoliated hBN barriers and epitaxially grown layers. The epitaxial barriers also exhibit enhanced conductance at localized subnanometer regions which are attributed to exposure of the substrate to a nitrogen plasma source during the high temperature growth process. Our results show clearly a spatial periodicity of tunnel current due to the formation of a moiré superlattice and we argue that this can provide a mechanism for elastic scattering of charge carriers for similar interfaces embedded in graphene/hBN resonant tunnel diodes.

Diamond and diamondlike carbon as wear-resistant, self-lubricating coatings for silicon nitride

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1995-01-01

Recent work on the friction and wear properties of as-deposited fine-grain diamond, polished coarse-grain diamond, and as-deposited diamondlike carbon (DLC) films in humid air at a relative humidity of approximately 40 percent and in dry nitrogen is reviewed. Two types of chemical vapor deposition (CVD) processes are used to deposit diamond films on silicon nitride (Si3N4) substrates: microwave-plasma and hot-filament. Ion beams are used to deposit DLC films of Si3N4 substrates. The diamond and DLC films in sliding contact with hemispherical bare Si3N4 pins have low steady-state coefficients of friction (less than 0.2) and low wear rates (less than 10(exp -7) mm(exp 2)/N-m), and thus, can be used effectively as wear-resistant, self-lubricating coatings for Si3N4 in the aforementioned two environments.

Group III-nitride thin films grown using MBE and bismuth

DOEpatents

Kisielowski, Christian K.; Rubin, Michael

2002-01-01

The present invention comprises growing gallium nitride films in the presence of bismuth using MBE at temperatures of about 1000 K or less. The present invention further comprises the gallium nitride films fabricated using the inventive fabrication method. The inventive films may be doped with magnesium or other dopants. The gallium nitride films were grown on sapphire substrates using a hollow anode Constricted Glow Discharge nitrogen plasma source. When bismuth was used as a surfactant, two-dimensional gallium nitride crystal sizes ranging between 10 .mu.m and 20 .mu.m were observed. This is 20 to 40 times larger than crystal sizes observed when GaN films were grown under similar circumstances but without bismuth. It is thought that the observed increase in crystal size is due bismuth inducing an increased surface diffusion coefficient for gallium. The calculated value of 4.7.times.10.sup.-7 cm.sup.2 /sec. reveals a virtual substrate temperature of 1258 K which is 260 degrees higher than the actual one.

Group III-nitride thin films grown using MBE and bismuth

DOEpatents

Kisielowski, Christian K.; Rubin, Michael

2000-01-01

The present invention comprises growing gallium nitride films in the presence of bismuth using MBE at temperatures of about 1000 K or less. The present invention further comprises the gallium nitride films fabricated using the inventive fabrication method. The inventive films may be doped with magnesium or other dopants. The gallium nitride films were grown on sapphire substrates using a hollow anode Constricted Glow Discharge nitrogen plasma source. When bismuth was used as a surfactant, two-dimensional gallium nitride crystal sizes ranging between 10 .mu.m and 20 .mu.m were observed. This is 20 to 40 times larger than crystal sizes observed when GaN films were grown under similar circumstances but without bismuth. It is thought that the observed increase in crystal size is due bismuth inducing an increased surface diffusion coefficient for gallium. The calculated value of 4.7.times.10.sup.-7 cm.sup.2 /sec. reveals a virtual substrate temperature of 1258 K which is 260 degrees higher than the actual one.

Tribological and microstructural characteristics of ion-nitrided steels

NASA Technical Reports Server (NTRS)

Spalvins, T.

1983-01-01

Three steels AISI 4140, AISI 4340 and AISI 304 stainless steel were ion nitrided in a plasma consisting of a 75:25 mixture of H2:N2, sometimes with a trace of CH4. Their surface topography was characterized by SEM and two distinct compound phases were identified: the gamma and the epsilon. The core-case hardness profiles were also established. The low Cr alloy steels have an extended diffusion zone in contrast to the 3034 stainless steels which have a sharp interface. The depth of ion-nitriding is increased as the Cr content is decreased. Friction tests reveal that the gamma surface phase has a lower coefficient of friction than the epsilon phase. The lowest coefficient of friction is achieved when both the rider and the specimen surface are ion nitrided. Previously announced in STAR as N83-24635

Structural tuning of residual conductivity in highly mismatched III-V layers

DOEpatents

Han, Jung; Figiel, Jeffrey J.

2002-01-01

A new process to control the electrical conductivity of gallium nitride layers grown on a sapphire substrate has been developed. This process is based on initially coating the sapphire substrate with a thin layer of aluminum nitride, then depositing the gallium nitride thereon. This process allows one to controllably produce gallium nitride layers with resistivity varying over as much as 10 orders of magnitude, without requiring the introduction and activation of suitable dopants.

One step process for producing dense aluminum nitride and composites thereof

DOEpatents

Holt, J.B.; Kingman, D.D.; Bianchini, G.M.

1989-10-31

A one step combustion process for the synthesis of dense aluminum nitride compositions is disclosed. The process comprises igniting pure aluminum powder in a nitrogen atmosphere at a pressure of about 1,000 atmospheres or higher. The process enables the production of aluminum nitride bodies to be formed directly in a mold of any desired shape.

One step process for producing dense aluminum nitride and composites thereof

DOEpatents

Holt, J. Birch; Kingman, Donald D.; Bianchini, Gregory M.

1989-01-01

A one step combustion process for the synthesis of dense aluminum nitride compositions is disclosed. The process comprises igniting pure aluminum powder in a nitrogen atmosphere at a pressure of about 1000 atmospheres or higher. The process enables the production of aluminum nitride bodies to be formed directly in a mold of any desired shape.

Electronic structure and mechanical properties of plasma nitrided ferrous alloys

NASA Astrophysics Data System (ADS)

Portolan, E.; Baumvol, I. J. R.; Figueroa, C. A.

2009-04-01

The electronic structures of the near-surface regions of two different nitrided steels (AISI 316 and 4140) were investigated using X-ray photoelectron spectroscopy. Photoelectron groups from all main chemical elements involved were addressed for steel samples with implanted-N concentrations in the range 16-32 at.%. As the implanted-N concentrations were increased, rather contrasting behaviors were observed for the two kinds of steel. The N1s photoelectrons had spectral shifts toward lower (nitrided AISI 316) or higher (nitrided AISI 4140) binding energies, whereas the Fe2p 3/2 photoelectron spectrum remains at a constant binding energy (nitrided AISI 316) or shifts toward higher binding energies (AISI 4140). These trends are discussed in terms of the metallic nitride formation and the overlapping of atomic orbitals. For nitrided AISI 316, a semi-classical approach of charge transfer between Cr and N is used to explain the experimental facts (formation of CrN), while for nitrided AISI 4140 we propose that the interaction between orbitals 4s from Fe and 2p from N promotes electrons to the conduction band increasing the electrical attraction of the N1s and Fe2p electrons in core shells (formation of FeN x). The increase in hardness of the steel upon N implantation is attributed to the localization of electrons in specific bonds, which diminishes the metallic bond character.

Research and Development for Continued Performance Improvement in Flexible a-Si PV

DTIC Science & Technology

2010-12-14

accomplished, however, at low temperatures silicides tend to form on the surface of the filament, which affected filament lifetime and deposition rate...considered. Titanium Nitride, sputtered As an alternative to the hot wire deposition of silicon, samples were prepared with various thicknesses of...Silicon 21 Insitu DC Sputtering Titanium Nitride 22 Metal Machine 2 ឈ> RF Oxygen Plasma Silicon Dioxide 20. Oxygen Etch Table A.4.1 Open circuit

Product surface hardening in non-self-sustained glow discharge plasma before synthesis of superhard coatings

NASA Astrophysics Data System (ADS)

Krasnov, P. S.; Metel, A. S.; Nay, H. A.

2017-05-01

Before the synthesis of superhard coating, the product surface is hardened by means of plasma nitriding, which prevents the surface deformations and the coating brittle rupture. The product heating by ions accelerated from plasma by applied to the product bias voltage leads to overheating and blunting of the product sharp edges. To prevent the blunting, it is proposed to heat the products with a broad beam of fast nitrogen molecules. The beam injection into a working vacuum chamber results in filling of the chamber with quite homogeneous plasma suitable for nitriding. Immersion in the plasma of the electrode and heightening of its potential up to 50-100 V initiate a non-self-sustained glow discharge between the electrode and the chamber. It enhances the plasma density by an order of magnitude and reduces its spatial nonuniformity down to 5-10%. When a cutting tool is isolated from the chamber, it is bombarded by plasma ions with an energy corresponding to its floating potential, which is lower than the sputtering threshold. Hence, the sharp edges are sputtered only by fast nitrogen molecules with the same rate as other parts of the tool surface. This leads to sharpening of the cutting tools instead of blunting.

A novel passivation process of silicon nanowires by a low-cost PECVD technique for deposition of hydrogenated silicon nitride using SiH4 and N2 as precursor gases

NASA Astrophysics Data System (ADS)

Bouaziz, Lamia; Dridi, Donia; Karyaoui, Mokhtar; Angelova, Todora; Sanchez Plaza, Guillermo; Chtourou, Radhouane

2017-03-01

In this work, a different SiNx passivation process of silicon nanowires has been opted for the deposition of a hydrogenated silicon nitride (SiNx:H) by a low-cost plasma enhanced chemical vapor deposition (PECVD) using silane ( SiH4 and nitrogen ( N2 as reactive gases. This study is focused on the effect of the gas flow ratio on chemical composition, morphological, optical and optoelectronic properties of silicon nanowires. The existence of Si-N and Si-H bonds was proven by the Fourier transmission infrared (FTIR) spectrum. Morphological structures were shown by scanning electron microscopy (SEM), and the roughness was investigated by atomic force microscopy (AFM). A low reflectivity less than 6% in the wavelength range 250-1200nm has been shown by UV-visible spectroscopy. Furthermore, the thickness and the refractive index of the passivation layer is determined by ellipsometry measurements. As a result, an improvement in minority carrier lifetime has been obtained by reducing surface recombination of silicon nanowires.

Group-III Nitride Field Emitters

NASA Technical Reports Server (NTRS)

Bensaoula, Abdelhak; Berishev, Igor

2008-01-01

Field-emission devices (cold cathodes) having low electron affinities can be fabricated through lattice-mismatched epitaxial growth of nitrides of elements from group III of the periodic table. Field emission of electrons from solid surfaces is typically utilized in vacuum microelectronic devices, including some display devices. The present field-emission devices and the method of fabricating them were developed to satisfy needs to reduce the cost of fabricating field emitters, make them compatible with established techniques for deposition of and on silicon, and enable monolithic integration of field emitters with silicon-based driving circuitry. In fabricating a device of this type, one deposits a nitride of one or more group-III elements on a substrate of (111) silicon or other suitable material. One example of a suitable deposition process is chemical vapor deposition in a reactor that contains plasma generated by use of electron cyclotron resonance. Under properly chosen growth conditions, the large mismatch between the crystal lattices of the substrate and the nitride causes strains to accumulate in the growing nitride film, such that the associated stresses cause the film to crack. The cracks lie in planes parallel to the direction of growth, so that the growing nitride film becomes divided into microscopic growing single-crystal columns. The outer ends of the fully-grown columns can serve as field-emission tips. By virtue of their chemical compositions and crystalline structures, the columns have low work functions and high electrical conductivities, both of which are desirable for field emission of electrons. From examination of transmission electron micrographs of a prototype device, the average column width was determined to be about 100 nm and the sharpness of the tips was determined to be characterized by a dimension somewhat less than 100 nm. The areal density of the columns was found to about 5 x 10(exp 9)/sq cm . about 4 to 5 orders of magnitude greater than the areal density of tips in prior field-emission devices. The electric field necessary to turn on the emission current and the current per tip in this device are both lower than in prior field-emission devices, such that it becomes possible to achieve longer operational lifetime. Moreover, notwithstanding the lower current per tip, because of the greater areal density of tips, it becomes possible to achieve greater current density averaged over the cathode area. The thickness of the grown nitride film (equivalently, the length of the columns) could lie between about 0.5 microns and a few microns; in any event, a thickness of about 1 micron is sufficient and costs less than do greater thicknesses. It may be possible to grow nitride emitter columns on glass or other substrate materials that cost less than silicon does. What is important in the choice of substrate material is the difference between the substrate and nitride crystalline structures. Inasmuch as the deposition process is nondestructive, an ability to grow emitter columns on a variety of materials would be advantageous in that it would facilitate the integration of field-emitter structures onto previously processed integrated circuits.

Homoepitaxial n-core: p-shell gallium nitride nanowires: HVPE overgrowth on MBE nanowires.

PubMed

Sanders, Aric; Blanchard, Paul; Bertness, Kris; Brubaker, Matthew; Dodson, Christopher; Harvey, Todd; Herrero, Andrew; Rourke, Devin; Schlager, John; Sanford, Norman; Chiaramonti, Ann N; Davydov, Albert; Motayed, Abhishek; Tsvetkov, Denis

2011-11-18

We present the homoepitaxial growth of p-type, magnesium doped gallium nitride shells by use of halide vapor phase epitaxy (HVPE) on n-type gallium nitride nanowires grown by plasma-assisted molecular beam epitaxy (MBE). Scanning electron microscopy shows clear dopant contrast between the core and shell of the nanowire. The growth of magnesium doped nanowire shells shows little or no effect on the lattice parameters of the underlying nanowires, as measured by x-ray diffraction (XRD). Photoluminescence measurements of the nanowires show the appearance of sub-bandgap features in the blue and the ultraviolet, indicating the presence of acceptors. Finally, electrical measurements confirm the presence of electrically active holes in the nanowires.

Silicon nitride films deposited with an electron beam created plasma

NASA Technical Reports Server (NTRS)

Bishop, D. C.; Emery, K. A.; Rocca, J. J.; Thompson, L. R.; Zamani, H.; Collins, G. J.

1984-01-01

The electron beam assisted chemical vapor deposition (EBCVD) of silicon nitride films using NH3, N2, and SiH4 as the reactant gases is reported. The films have been deposited on aluminum, SiO2, and polysilicon film substrates as well as on crystalline silicon substrates. The range of experimental conditions under which silicon nitrides have been deposited includes substrate temperatures from 50 to 400 C, electron beam currents of 2-40 mA, electron beam energies of 1-5 keV, total ambient pressures of 0.1-0.4 Torr, and NH3/SiH4 mass flow ratios of 1-80. The physical, electrical, and chemical properties of the EBCVD films are discussed.

Coating for components requiring hydrogen peroxide compatibility

NASA Technical Reports Server (NTRS)

Yousefiani, Ali (Inventor)

2010-01-01

The present invention provides a heretofore-unknown use for zirconium nitride as a hydrogen peroxide compatible protective coating that was discovered to be useful to protect components that catalyze the decomposition of hydrogen peroxide or corrode when exposed to hydrogen peroxide. A zirconium nitride coating of the invention may be applied to a variety of substrates (e.g., metals) using art-recognized techniques, such as plasma vapor deposition. The present invention further provides components and articles of manufacture having hydrogen peroxide compatibility, particularly components for use in aerospace and industrial manufacturing applications. The zirconium nitride barrier coating of the invention provides protection from corrosion by reaction with hydrogen peroxide, as well as prevention of hydrogen peroxide decomposition.

High density hexagonal boron nitride prepared by hot isostatic pressing in refractory metal containers

DOEpatents

Hoenig, Clarence L.

1992-01-01

Boron nitride powder with less than or equal to the oxygen content of starting powder (down to 0.5% or less) is hot isostatically pressed in a refractory metal container to produce hexagonal boron nitride with a bulk density greater than 2.0 g/cc. The refractory metal container is formed of tantalum, niobium, tungsten, molybdenum or alloys thereof in the form of a canister or alternatively plasma sprayed or chemical vapor deposited onto a powder compact. Hot isostatic pressing at 1800.degree. C. and 30 KSI (206.8 MPa) argon pressure for four hours produces a bulk density of 2.21 g/cc. Complex shapes can be made.

Fabrication of Antireflective Sub-Wavelength Structures on Silicon Nitride Using Nano Cluster Mask for Solar Cell Application

PubMed Central

2009-01-01

We have developed a simple and scalable approach for fabricating sub-wavelength structures (SWS) on silicon nitride by means of self-assembled nickel nanoparticle masks and inductively coupled plasma (ICP) ion etching. Silicon nitride SWS surfaces with diameter of 160–200 nm and a height of 140–150 nm were obtained. A low reflectivity below 1% was observed over wavelength from 590 to 680 nm. Using the measured reflectivity data in PC1D, the solar cell characteristics has been compared for single layer anti-reflection (SLAR) coatings and SWS and a 0.8% improvement in efficiency has been seen. PMID:20596409

Tuning Material Properties of Oxides and Nitrides by Substrate Biasing during Plasma-Enhanced Atomic Layer Deposition on Planar and 3D Substrate Topographies.

PubMed

Faraz, Tahsin; Knoops, Harm C M; Verheijen, Marcel A; van Helvoirt, Cristian A A; Karwal, Saurabh; Sharma, Akhil; Beladiya, Vivek; Szeghalmi, Adriana; Hausmann, Dennis M; Henri, Jon; Creatore, Mariadriana; Kessels, Wilhelmus M M

2018-04-18

Oxide and nitride thin-films of Ti, Hf, and Si serve numerous applications owing to the diverse range of their material properties. It is therefore imperative to have proper control over these properties during materials processing. Ion-surface interactions during plasma processing techniques can influence the properties of a growing film. In this work, we investigated the effects of controlling ion characteristics (energy, dose) on the properties of the aforementioned materials during plasma-enhanced atomic layer deposition (PEALD) on planar and 3D substrate topographies. We used a 200 mm remote PEALD system equipped with substrate biasing to control the energy and dose of ions by varying the magnitude and duration of the applied bias, respectively, during plasma exposure. Implementing substrate biasing in these forms enhanced PEALD process capability by providing two additional parameters for tuning a wide range of material properties. Below the regimes of ion-induced degradation, enhancing ion energies with substrate biasing during PEALD increased the refractive index and mass density of TiO x and HfO x and enabled control over their crystalline properties. PEALD of these oxides with substrate biasing at 150 °C led to the formation of crystalline material at the low temperature, which would otherwise yield amorphous films for deposition without biasing. Enhanced ion energies drastically reduced the resistivity of conductive TiN x and HfN x films. Furthermore, biasing during PEALD enabled the residual stress of these materials to be altered from tensile to compressive. The properties of SiO x were slightly improved whereas those of SiN x were degraded as a function of substrate biasing. PEALD on 3D trench nanostructures with biasing induced differing film properties at different regions of the 3D substrate. On the basis of the results presented herein, prospects afforded by the implementation of this technique during PEALD, such as enabling new routes for topographically selective deposition on 3D substrates, are discussed.

Work functions of hafnium nitride thin films as emitter material for field emitter arrays

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gotoh, Yasuhito, E-mail: gotoh.yasuhito.5w@kyoto-u.ac.jp; Fujiwara, Sho; Tsuji, Hiroshi

The work functions of hafnium nitride thin films prepared by radio-frequency magnetron sputtering were investigated in vacuum, before and after surface cleaning processes, with a view of improving the properties of as-fabricated field emitter arrays comprising hafnium nitride emitters. The measurement of the work function was first performed for the as-deposited films and then for films subjected to surface cleaning process, either thermal treatment or ion bombardment. Thermal treatment at a maximum temperature of 300 °C reduced the work function by 0.7 eV. Once the film was heated, the work function maintained the reduced value, even after cooling to room temperature. Amore » little change in the work function was observed for the second and third thermal treatments. The ion bombardment was conducted by exposing the sample to a thin plasma for different sample bias conditions and processing times. When the sample was biased at −10 V, the work function decreased by 0.6 eV. The work function reduction became saturated in the early stage of the ion bombardment. When the sample was biased at −50 V, the work function exhibited different behaviors, that is, first it decreased rapidly and then increased in response to the increase in processing time. The lowest attainable work function was found to be 4.00 eV. It should be noted that none of the work function values reported in this paper were obtained using surfaces that were demonstrated to be free from oxygen contamination. The present results suggest that the current–voltage characteristics of a field emitter array can be improved by a factor of 25–50 by the examined postprocesses.« less

Plasma chemistry for inorganic materials

NASA Technical Reports Server (NTRS)

Matsumoto, O.

1980-01-01

Practical application of plasma chemistry to the development of inorganic materials using both low temperature and warm plasmas are summarized. Topics cover: the surface nitrification and oxidation of metals; chemical vapor deposition; formation of minute oxide particles; the composition of oxides from chloride vapor; the composition of carbides and nitrides; freezing high temperature phases by plasma arc welding and plasma jet; use of plasma in the development of a substitute for petroleum; the production of silicon for use in solar cell batteries; and insulating the inner surface of nuclear fusion reactor walls.

Frictional and structural characterization of ion-nitrided low and high chromium steels

NASA Technical Reports Server (NTRS)

Spalvins, T.

1985-01-01

Low Cr steels AISI 41410, AISI 4340, and high Cr austenitic stainless steels AISI 304, AISI 316 were ion nitrided in a dc glow discharge plasma consisting of a 75 percent H2 - 25 percent N2 mixture. Surface compound layer phases were identified, and compound layer microhardness and diffusion zone microhardness profiles were established. Distinct differences in surface compound layer hardness and diffusion zone profiles were determined between the low and high Cr alloy steels. The high Cr stainless steels after ion nitriding displayed a hard compound layer and an abrupt diffusion zone. The compound layers of the high Cr stainless steels had a columnar structure which accounts for brittleness when layers are exposed to contact stresses. The ion nitrided surfaces of high and low Cr steels displayed a low coefficient of friction with respect to the untreated surfaces when examined in a pin and disk tribotester.

Thin films of aluminum nitride and aluminum gallium nitride for cold cathode applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sowers, A.T.; Christman, J.A.; Bremser, M.D.

1997-10-01

Cold cathode structures have been fabricated using AlN and graded AlGaN structures (deposited on n-type 6H-SiC) as the thin film emitting layer. The cathodes consist of an aluminum grid layer separated from the nitride layer by a SiO{sub 2} layer and etched to form arrays of either 1, 3, or 5 {mu}m holes through which the emitting nitride surface is exposed. After fabrication, a hydrogen plasma exposure was employed to activate the cathodes. Cathode devices with 5 {mu}m holes displayed emission for up to 30 min before failing. Maximum emission currents ranged from 10{endash}100 nA and required grid voltages rangingmore » from 20{endash}110 V. The grid currents were typically 1 to 10{sup 4} times the collector currents. {copyright} {ital 1997 American Institute of Physics.}« less

Alloy Effects on the Gas Nitriding Process

NASA Astrophysics Data System (ADS)

Yang, M.; Sisson, R. D.

2014-12-01

Alloy elements, such as Al, Cr, V, and Mo, have been used to improve the nitriding performance of steels. In the present work, plain carbon steel AISI 1045 and alloy steel AISI 4140 were selected to compare the nitriding effects of the alloying elements in AISI 4140. Fundamental analysis is carried out by using the "Lehrer-like" diagrams (alloy specific Lehrer diagram and nitriding potential versus nitrogen concentration diagram) and the compound layer growth model to simulate the gas nitriding process. With this method, the fundamental understanding for the alloy effect based on the thermodynamics and kinetics becomes possible. This new method paves the way for the development of new alloy for nitriding.

Dispersible shortened boron nitride nanotubes with improved molecule-loading capacity.

PubMed

Zhi, Chunyi; Hanagata, Nobutaka; Bando, Yoshio; Golberg, Dmitri

2011-09-05

The oxidation process of boron nitride nanotubes was thoroughly investigated, and a slow oxidation characteristic was clearly revealed. Subsequently, the controllable oxidation process was utilized to break the sturdy structure of the boron nitride nanotubes to fabricate shortened nanotubes. The shortened boron nitride nanotubes were found to possess good solubility in water and many organic solvents. Further experiments demonstrated remarkably improved molecule-loading capacity of the shortened boron nitride nanotubes. These dispersible shortened boron nitride nanotubes might have the potential to be developed as effective delivery systems for various molecules, which may find applications in bio-related fields. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Low temperature synthesis of silicon quantum dots with plasma chemistry control in dual frequency non-thermal plasmas.

PubMed

Sahu, Bibhuti Bhusan; Yin, Yongyi; Han, Jeon Geon; Shiratani, Masaharu

2016-06-21

The advanced materials process by non-thermal plasmas with a high plasma density allows the synthesis of small-to-big sized Si quantum dots by combining low-temperature deposition with superior crystalline quality in the background of an amorphous hydrogenated silicon nitride matrix. Here, we make quantum dot thin films in a reactive mixture of ammonia/silane/hydrogen utilizing dual-frequency capacitively coupled plasmas with high atomic hydrogen and nitrogen radical densities. Systematic data analysis using different film and plasma characterization tools reveals that the quantum dots with different sizes exhibit size dependent film properties, which are sensitively dependent on plasma characteristics. These films exhibit intense photoluminescence in the visible range with violet to orange colors and with narrow to broad widths (∼0.3-0.9 eV). The observed luminescence behavior can come from the quantum confinement effect, quasi-direct band-to-band recombination, and variation of atomic hydrogen and nitrogen radicals in the film growth network. The high luminescence yields in the visible range of the spectrum and size-tunable low-temperature synthesis with plasma and radical control make these quantum dot films good candidates for light emitting applications.

Characterization of DC Magnetron Sputtering Plasma Used for Deposition of Amorphous Carbon Nitride

NASA Astrophysics Data System (ADS)

Camps, Enrique; Escobar-Alarcón, Luis; López, J.; Zambrano, G.; Prieto, P.

2006-12-01

Amorphous carbon nitride (a-CNx) thin films are attractive due to their potential applications, in different areas. This material can be hard and used as a protective coating, or can be soft and porous and used as the active element in gas sensors, it can also be used as a radiation detector due to its thermoluminescent response. The use of this material for one or another application, will depend on the material's structure, which can be changed by changing the deposition parameters. When using the d.c. magnetron sputtering technique it means mainly the change of discharge power, type of Ar/N2 gas mixture, and the working gas pressure. The variation of these deposition parameters has an important influence on the characteristics of the plasma formed in the discharge. In this work we studied the plasma characteristics, such as the type of excited species, plasma density, and electron temperature under different deposition conditions, using Optical Emission Spectroscopy (OES), and a single Langmuir probe. These parameters were correlated with the properties of a-CNx films deposited under those characterized regimes, in order to establish the role that the plasma parameters play on the formation of the different structures of CNx films.

Chemically Adjusting Plasma Temperature, Energy and Reactivity (CAPTEAR) Method Using NOx and Combustion for Selective Synthesis of Sc3N@C80 Metallic Nitride Fullerenes

PubMed Central

Stevenson, Steven; Thompson, M. Corey; Coumbe, H. Louie; Mackey, Mary A.; Coumbe, Curtis E.; Phillips, J. Paige

2008-01-01

Goals are (1) to selectively synthesize MNFs in lieu of empty-cage fullerenes (e.g., C60, C70) without compromising MNF yield and (2) to test our hypothesis that MNFs possess a different set of optimal formation parameters than empty-cage fullerenes. In this work, we introduce a novel approach for the selective synthesis of metallic nitride fullerenes (MNFs). This new method is “Chemically Adjusting Plasma Temperature, Energy and Reactivity” (CAPTEAR). The CAPTEAR approach with copper nitrate hydrate uses NOx vapor from NOx generating solid reagents, air and combustion to “tune” the temperature, energy and reactivity of the plasma environment. The extent of temperature, energy and reactive environment is stoichiometrically varied until optimal conditions for selective MNF synthesis are achieved. Analysis of soot extracts indicate that percentages of C60 and Sc3N@C80 are inversely related, whereas the percentages of C70 and higher empty-cage C2n fullerenes are largely unaffected. Hence, there may be a “competitive link” in the formation and mechanism of C60 and Sc3N@C80. Using this CAPTEAR method, purified MNFs (96% Sc3N@C80, 12 mg) have been obtained in soot extracts without a significant penalty in milligram yield when compared to control soot extracts (4% Sc3N@C80, 13 mg Sc3N@C80). The CAPTEAR process with Cu(NO3)2·2.5 H2O uses an exothermic nitrate moiety to suppress empty-cage fullerene formation, whereas Cu functions as a catalyst additive to offset the reactive plasma environment and boost the Sc3N@C80 MNF production. PMID:18052069

Aaron Ptak | NREL

Science.gov Websites

doping of III-Nitride materials grown by molecular beam epitaxy (MBE). He joined NREL after graduation in (0001) GaN Growth by Radio Frequency Plasma-Assisted Molecular Beam Epitaxy, A.J. Ptak, M.R. Millecchia . Phys. Lett. 77, 2479 (2000). Magnesium Incorporation in GaN Grown by rf-Plasma Assisted Molecular Beam

A method to monitor the quality of ultra-thin nitride for trench DRAM with a buried strap structure

NASA Astrophysics Data System (ADS)

Wu, Yung-Hsien; Wang, Chun-Yao; Chang, Ian; Kao, Chien-Kang; Kuo, Chia-Ming; Ku, Alex

2007-02-01

A new approach to monitor the quality of an ultra-thin nitride film has been proposed. The nitride quality is monitored by observing the oxide thickness for the nitride film after wet oxidation since the resistance to oxidation strongly depends on its quality. To obtain a stable oxide thickness without interference from extrinsic factors for process monitoring, monitor wafers without dilute HF solution clean are suggested because the native-oxide containing surface is less sensitive to oxygen and therefore forms the nitride film with stable quality. In addition, the correlation between variable retention time (VRT) performance of a real dynamic random access memory (DRAM) product and oxide thickness from different nitride process temperatures can be successfully explained and this correlation can also be used to establish the appropriate oxide thickness range for process monitoring.

Interface trap and oxide charge generation under negative bias temperature instability of p-channel metal-oxide-semiconductor field-effect transistors with ultrathin plasma-nitrided SiON gate dielectrics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu Shiyang; Nakajima, Anri; Ohashi, Takuo

2005-12-01

The interface trap generation ({delta}N{sub it}) and fixed oxide charge buildup ({delta}N{sub ot}) under negative bias temperature instability (NBTI) of p-channel metal-oxide-semiconductor field-effect transistors (pMOSFETs) with ultrathin (2 nm) plasma-nitrided SiON gate dielectrics were studied using a modified direct-current-current-voltage method and a conventional subthreshold characteristic measurement. Different stress time dependences were shown for {delta}N{sub it} and {delta}N{sub ot}. At the earlier stress times, {delta}N{sub it} dominates the threshold voltage shift ({delta}V{sub th}) and {delta}N{sub ot} is negligible. With increasing stress time, the rate of increase of {delta}N{sub it} decreases continuously, showing a saturating trend for longer stress times, while {delta}N{submore » ot} still has a power-law dependence on stress time so that the relative contribution of {delta}N{sub ot} increases. The thermal activation energy of {delta}N{sub it} and the NBTI lifetime of pMOSFETs, compared at a given stress voltage, are independent of the peak nitrogen concentration of the SiON film. This indicates that plasma nitridation is a more reliable method for incorporating nitrogen in the gate oxide.« less

Characterization of Ar/N2/H2 middle-pressure RF discharge and application of the afterglow region for nitridation of GaAs

NASA Astrophysics Data System (ADS)

Raud, J.; Jõgi, I.; Matisen, L.; Navrátil, Z.; Talviste, R.; Trunec, D.; Aarik, J.

2017-12-01

This work characterizes the production and destruction of nitrogen and hydrogen atoms in RF capacitively coupled middle-pressure discharge in argon/nitrogen/hydrogen mixtures. Input power, electron concentration, electric field strength and mean electron energy were determined on the basis of electrical measurements. Gas temperature and concentration of Ar atoms in 1s states were determined from spectral measurements. On the basis of experimentally determined plasma characteristics, main production and loss mechanisms of H and N atoms were discussed. The plasma produced radicals were applied for the nitridation and oxide reduction of gallium arsenide in the afterglow region of discharge. After plasma treatment the GaAs samples were analyzed using x-ray photoelectron spectroscopy (XPS) technique. Successful nitridation of GaAs sample was obtained in the case of Ar/5% N2 discharge. In this gas mixture the N atoms were generated via dissociative recombination of N2+ created by charge transfer from Ar+. The treatment in Ar/5% N2/1% H2 mixture resulted in the reduction of oxide signals in the XPS spectra. Negligible formation of GaN in the latter mixture was connected with reduced concentration of N atoms, which was, in turn, due to less efficient mechanism of N atom production (electron impact dissociation of N2 molecules) and additional loss channel in reaction with H2.

Influence of low energy argon plasma treatment on the moisture barrier performance of hot wire-CVD grown SiNx multilayers

NASA Astrophysics Data System (ADS)

Majee, Subimal; Fátima Cerqueira, Maria; Tondelier, Denis; Geffroy, Bernard; Bonnassieux, Yvan; Alpuim, Pedro; Bourée, Jean Eric

2014-01-01

The reliability and stability are key issues for the commercial utilization of organic photovoltaic devices based on flexible polymer substrates. To increase the shelf-lifetime of these devices, transparent moisture barriers of silicon nitride (SiNx) films are deposited at low temperature by hot wire CVD (HW-CVD) process. Instead of the conventional route based on organic/inorganic hybrid structures, this work defines a new route consisting in depositing multilayer stacks of SiNx thin films, each single layer being treated by argon plasma. The plasma treatment allows creating smoother surface and surface atom rearrangement. We define a critical thickness of the single layer film and focus our attention on the effect of increasing the number of SiNx single-layers on the barrier properties. A water vapor transmission rate (WVTR) of 2 × 10-4 g/(m2·day) is reported for SiNx multilayer stack and a physical interpretation of the plasma treatment effect is given.

Reflection high energy electron diffraction study of nitrogen plasma interactions with a GaAs (100) surface

NASA Astrophysics Data System (ADS)

Hauenstein, R. J.; Collins, D. A.; Cai, X. P.; O'Steen, M. L.; McGill, T. C.

1995-05-01

Effect of a nitrogen electron-cyclotron-resonance (ECR) microwave plasma on near-surface composition, crystal structure, and morphology of the As-stabilized GaAs (100) surface is investigated with the use of digitally image-processed in situ reflection high energy electron diffraction. Nitridation is performed on molecular beam epitaxially (MBE) grown GaAs surfaces near 600 °C under typical conditions for ECR microwave plasma-assisted MBE growth of GaN films on GaAs. Brief plasma exposures (≊3-5 s) are shown to result in a specular, coherently strained, relatively stable, GaN film approximately one monolayer in thickness, which can be commensurately overgrown with GaAs while longer exposures (up to 1 min) result in incommensurate zincblende epitaxial GaN island structures. Specular and nonspecular film formations are explained in terms of N-for-As surface and subsurface anion exchange reactions, respectively. Commensurate growth of ultrathin buried GaN layers in GaAs is achieved.

Process for producing ceramic nitrides anc carbonitrides and their precursors

DOEpatents

Brown, G.M.; Maya, L.

1987-02-25

A process for preparing ceramic nitrides and carbon nitrides in the form of very pure, fine particulate powder. Appropriate precursors is prepared by reaching a transition metal alkylamide with ammonia to produce a mixture of metal amide and metal imide in the form of an easily pyrolyzable precipitate.

Electronic and Optical Properties of Titanium Nitride Bulk and Surfaces from First Principles Calculations (Postprint)

DTIC Science & Technology

2015-11-18

thickness of the film, or substrate. In this work, we report calculations for titanium nitride ( TiN ), a promising material for plasmonic applications...stoichiometric bulk TiN , as well as of the TiN (100), TiN (110), and TiN (111) outermost surfaces. Density functional theory (DFT) and many-body GW methods...and the band structure for bulk TiN were shown to be consistent with previous work. Calculated dielectric functions, plasma frequencies, reflectivity

Behaviors of Absolute Densities of N, H, and NH3 at Remote Region of High-Density Radical Source Employing N2-H2 Mixture Plasmas

NASA Astrophysics Data System (ADS)

Chen, Shang; Kondo, Hiroki; Ishikawa, Kenji; Takeda, Keigo; Sekine, Makoto; Kano, Hiroyuki; Den, Shoji; Hori, Masaru

2011-01-01

For an innovation of molecular-beam-epitaxial (MBE) growth of gallium nitride (GaN), the measurements of absolute densities of N, H, and NH3 at the remote region of the radical source excited by plasmas have become absolutely imperative. By vacuum ultraviolet absorption spectroscopy (VUVAS) at a relatively low pressure of about 1 Pa, we obtained a N atom density of 9×1012 cm-3 for a pure nitrogen gas used, a H atom density of 7×1012 cm-3 for a gas composition of 80% hydrogen mixed with nitrogen gas were measured. The maximum density 2×1013 cm-3 of NH3 was measured by quadruple mass spectrometry (QMS) at H2/(N2+H2)=60%. Moreover, we found that N atom density was considerably affected by processing history, where the characteristic instability was observed during the pure nitrogen plasma discharge sequentially after the hydrogen-containing plasma discharge. These results indicate imply the importance of establishing radical-based processes to control precisely the absolute densities of N, H, and NH3 at the remote region of the radical source.

Synthesis of nano-structure tungsten nitride thin films on silicon using Mather-type plasma focus

NASA Astrophysics Data System (ADS)

Hussnain, A.; Rawat, R. S.; Ahmad, R.; Umar, Z. A.; Hussain, T.; Lee, P.; Chen, Z.

2015-07-01

Nano-structure thin film of tungsten nitride was deposited onto Si-substrate at room temperature using Mather-type plasma focus (3.3 kJ) machine. Substrate was exposed against 10, 20, 30, and 40 deposition shots and its corresponding effect on structure, morphology, conductivity and nano-hardness has been systematically studied. The X-ray diffractormeter spectra of the exposed samples show the presence of various phases of WN and WN2 that depends on number of deposition shots. Surface morphological study revealed the uniform distribution of nano-sized grains on deposited film surface. Hardness and conductivity of exposed substrate improved with higher deposition shots. X-ray photo-electron spectroscopy survey scan of 40 deposition shots confirmed the elemental presence of W and N on Si-substrate.

High-Performance and Self-Powered Deep UV Photodetectors Based on High Quality 2D Boron Nitride Nanosheets

PubMed Central

Rivera, Manuel; Rahaman, Mostafizur; Zhou, Andrew F.; Mohammed Alzuraiqi, Waleed; Feng, Peter

2017-01-01

High-quality two-dimensional (2D) crystalline boron nitride nanosheets (BNNSs) were grown on silicon wafers by using pulsed plasma beam deposition techniques. Self-powered deep ultraviolet (DUV) photodetectors (PDs) based on BNNSs with Schottky contact structures are designed and fabricated. By connecting the fabricated DUV photodetector to an ammeter, the response strength, response time and recovery time to different DUV wavelengths at different intensities have been characterized using the output short circuit photocurrent without a power supply. Furthermore, effects of temperature and plasma treatment on the induced photocurrent response of detectors have also been investigated. The experimental data clearly indicate that plasma treatment would significantly improve both induced photocurrent and response time. The BNNS-based DUV photodetector is demonstrated to possess excellent performance at a temperature up to 400 °C, including high sensitivity, high signal-to-noise ratio, high spectral selectivity, high speed, and high stability, which is better than almost all reported semiconducting nanomaterial-based self-powered photodetectors. PMID:29257098

Fabrication of (NH4)2S passivated GaAs metal-insulator-semiconductor devices using low-frequency plasma-enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Jaouad, A.; Aimez, V.; Aktik, Ç.; Bellatreche, K.; Souifi, A.

2004-05-01

Metal-insulator-semiconductor (MIS) capacitors were fabricated on n-GaAs(100) substrate using (NH4)2S surface passivation and low-frequency plasma-enhanced chemical vapor deposited silicon nitride as gate insulators. The electrical properties of the fabricated MIS capacitors were analyzed using high-frequency capacitance-voltage and conductance-voltage measurements. The high concentration of hydrogen present during low-frequency plasma deposition of silicon nitride enhances the passivation of GaAs surface, leading to the unpinning of the Fermi level and to a good modulation of the surface potential by gate voltage. The electrical properties of the insulator-semiconductor interface are improved after annealing at 450 °C for 60 s, as a significant reduction of the interface fixed charges and of the interface states density is put into evidence. The minimum interface states density was found to be about 3×1011 cm-2 eV-1, as estimated by the Terman method. .

Molten tin reprocessing of spent nuclear fuel elements. [Patent application; continuous process

DOEpatents

Heckman, R.A.

1980-12-19

A method and apparatus for reprocessing spent nuclear fuel is described. Within a containment vessel, a solid plug of tin and nitride precipitates supports a circulating bath of liquid tin therein. Spent nuclear fuel is immersed in the liquid tin under an atmosphere of nitrogen, resulting in the formation of nitride precipitates. The layer of liquid tin and nitride precipitates which interfaces the plug is solidified and integrated with the plug. Part of the plug is melted, removing nitride precipitates from the containment vessel, while a portion of the plug remains solidified to support te liquid tin and nitride precipitates remaining in the containment vessel. The process is practiced numerous times until substantially all of the precipitated nitrides are removed from the containment vessel.

Review: engineering particles using the aerosol-through-plasma method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Phillips, Jonathan; Luhrs, Claudia C; Richard, Monique

2009-01-01

For decades, plasma processing of materials on the nanoscale has been an underlying enabling technology for many 'planar' technologies, particularly virtually every aspect of modern electronics from integrated-circuit fabrication with nanoscale elements to the newest generation of photovoltaics. However, it is only recent developments that suggest that plasma processing can be used to make 'particulate' structures of value in fields, including catalysis, drug delivery, imaging, higher energy density batteries, and other forms of energy storage. In this paper, the development of the science and technology of one class of plasma production of particulates, namely, aerosol-through-plasma (A-T-P), is reviewed. Various plasmamore » systems, particularly RF and microwave, have been used to create nanoparticles of metals and ceramics, as well as supported metal catalysts. Gradually, the complexity of the nanoparticles, and concomitantly their potential value, has increased. First, unique two-layer particles were generated. These were postprocessed to create unique three-layer nanoscale particles. Also, the technique has been successfully employed to make other high-value materials, including carbon nanotubes, unsupported graphene, and spherical boron nitride. Some interesting plasma science has also emerged from efforts to characterize and map aerosol-containing plasmas. For example, it is clear that even a very low concentration of particles dramatically changes plasma characteristics. Some have also argued that the local-thermodynamic-equilibrium approach is inappropriate to these systems. Instead, it has been suggested that charged- and neutral-species models must be independently developed and allowed to 'interact' only in generation terms.« less

Nitride stabilized core/shell nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kuttiyiel, Kurian Abraham; Sasaki, Kotaro; Adzic, Radoslav R.

Nitride stabilized metal nanoparticles and methods for their manufacture are disclosed. In one embodiment the metal nanoparticles have a continuous and nonporous noble metal shell with a nitride-stabilized non-noble metal core. The nitride-stabilized core provides a stabilizing effect under high oxidizing conditions suppressing the noble metal dissolution during potential cycling. The nitride stabilized nanoparticles may be fabricated by a process in which a core is coated with a shell layer that encapsulates the entire core. Introduction of nitrogen into the core by annealing produces metal nitride(s) that are less susceptible to dissolution during potential cycling under high oxidizing conditions.

Kinetic modeling of microscopic processes during electron cyclotron resonance microwave plasma-assisted molecular beam epitaxial growth of GaN/GaAs-based heterostructures

NASA Astrophysics Data System (ADS)

Bandić, Z. Z.; Hauenstein, R. J.; O'Steen, M. L.; McGill, T. C.

1996-03-01

Microscopic growth processes associated with GaN/GaAs molecular beam epitaxy (MBE) are examined through the introduction of a first-order kinetic model. The model is applied to the electron cyclotron resonance microwave plasma-assisted MBE (ECR-MBE) growth of a set of δ-GaNyAs1-y/GaAs strained-layer superlattices that consist of nitrided GaAs monolayers separated by GaAs spacers, and that exhibit a strong decrease of y with increasing T over the range 540-580 °C. This y(T) dependence is quantitatively explained in terms of microscopic anion exchange, and thermally activated N surface-desorption and surface-segregation processes. N surface segregation is found to be significant during GaAs overgrowth of GaNyAs1-y layers at typical GaN ECR-MBE growth temperatures, with an estimated activation energy Es˜0.9 eV. The observed y(T) dependence is shown to result from a combination of N surface segregation/desorption processes.

Direct growth of graphene on in situ epitaxial hexagonal boron nitride flakes by plasma-assisted molecular beam epitaxy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Zhongguang; Zheng, Renjing; Khanaki, Alireza

2015-11-23

Hexagonal boron nitride (h-BN) single-crystal domains were grown on cobalt (Co) substrates at a substrate temperature of 850–900 °C using plasma-assisted molecular beam epitaxy. Three-point star shape h-BN domains were observed by scanning electron microscopy, and confirmed by Raman and X-ray photoelectron spectroscopy. The h-BN on Co template was used for in situ growth of multilayer graphene, leading to an h-BN/graphene heterostructure. Carbon atoms preferentially nucleate on Co substrate and edges of h-BN and then grow laterally to form continuous graphene. Further introduction of carbon atoms results in layer-by-layer growth of graphene on graphene and lateral growth of graphene on h-BNmore » until it may cover entire h-BN flakes.« less

A study of structural and mechanical properties of nano-crystalline tungsten nitride film synthesis by plasma focus

NASA Astrophysics Data System (ADS)

Hussnain, Ali; Singh Rawat, Rajdeep; Ahmad, Riaz; Hussain, Tousif; Umar, Z. A.; Ikhlaq, Uzma; Chen, Zhong; Shen, Lu

2015-02-01

Nano-crystalline tungsten nitride thin films are synthesized on AISI-304 steel at room temperature using Mather-type plasma focus system. The surface properties of the exposed substrate against different deposition shots are examined for crystal structure, surface morphology and mechanical properties using X-ray diffraction (XRD), atomic force microscope, field emission scanning electron microscope and nano-indenter. The XRD results show the growth of WN and WN2 phases and the development of strain/stress in the deposited films by varying the number of deposition shots. Morphology of deposited films shows the significant change in the surface structure with different ion energy doses (number of deposition shots). Due to the effect of different ion energy doses, the strain/stress developed in the deposited film leads to an improvement of hardness of deposited films.

Increasing Wear Resistance of Titanium Alloys by Anode Plasma Electrolytic Saturation with Interstitial Elements

NASA Astrophysics Data System (ADS)

Belkin, P. N.; Kusmanov, S. A.; Dyakov, I. G.; Silkin, S. A.; Smirnov, A. A.

2017-05-01

In our previous studies, we have shown that anode plasma electrolytic saturation of titanium alloys with nitrogen and carbon can improve their tribological properties. Obtained structure containing oxide layer and solid solution of diffused element in titanium promotes the enhancement of running-in ability and the decrease in the wear rate in some special cases. In this paper, further investigations are reported regarding the tribological properties of alpha- and beta-titanium alloys in wear test against hardened steel (50 HRC) disk using pin-on-disk geometry and balls of Al2O3 (6.25 mm in diameter) or bearing steel (9.6 mm in diameter) with ball-on-plate one and normal load from 5 to 209 N. Reproducible results were obtained under testing samples treated by means of the plasma electrolytic nitriding (PEN) with the mechanical removal of the oxide layer. Friction coefficient of nitrided samples is 0.5-0.9 which is somewhat higher than that for untreated one (0.48-0.75) during dry sliding against Al2O3 ball. An increase in the sliding speed results in the polishing of nitrided samples and reduction of their wear rate by 60 times. This result is obtained for 5 min at 850 °C using PEN in electrolyte containing 5 wt.% ammonia and 10 wt.% ammonium chloride followed by quenching in solution. Optical microscope was employed to assist in the evaluation of the wear behavior. Sizes of wear tracks were measured by profilometer TR200.

Surface Chemistry, Microstructure, and Tribological Properties of Cubic Boron Nitride Films

NASA Technical Reports Server (NTRS)

Watanabe, Shuichi; Wheeler, Donald R.; Abel, Phillip B.; Street, Kenneth W.; Miyoshi, Kazuhisa; Murakawa, Masao; Miyake, Shojiro

1998-01-01

This report deals with the surface chemistry, microstructure, bonding state, morphology, and friction and wear properties of cubic boron nitride (c-BN) films that were synthesized by magnetically enhanced plasma ion plating. Several analytical techniques - x-ray photoelectron spectroscopy, transmission electron microscopy and electron diffraction, Fourier transform infrared spectroscopy, atomic force microscopy, and surface profilometry - were used to characterize the films. Sliding friction experiments using a ball-on-disk configuration were conducted for the c-BN films in sliding contact with 440C stainless-steel balls at room temperature in ultrahigh vacuum (pressure, 10(exp -6), in ambient air, and under water lubrication. Results indicate that the boron-to-nitrogen ratio on the surface of the as-deposited c-BN film is greater than 1 and that not all the boron is present as boron nitride but a small percentage is present as an oxide. Both in air and under water lubrication, the c-BN film in sliding contact with steel showed a low wear rate, whereas a high wear rate was observed in vacuum. In air and under water lubrication, c-BN exhibited wear resistance superior to that of amorphous boron nitride, titanium nitride, and titanium carbide.

Surface cleaning for enhanced adhesion to packaging surfaces: Effect of oxygen and ammonia plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gaddam, Sneha; Dong, Bin; Driver, Marcus

2015-03-15

The effects of direct plasma chemistries on carbon removal from silicon nitride (SiN{sub x}) and oxynitride (SiO{sub x}N{sub y}) surfaces have been studied by in-situ x-ray photoelectron spectroscopy (XPS) and ex-situ contact angle measurements. The data indicate that O{sub 2} and NH{sub 3} capacitively coupled plasmas are effective at removing adventitious carbon from silicon nitride (SiN{sub x}) and Si oxynitride (SiO{sub x}N{sub y}) surfaces. O{sub 2} plasma treatment results in the formation of a silica overlayer. In contrast, the exposure to NH{sub 3} plasma results in negligible additional oxidation of the SiN{sub x} or SiO{sub x}N{sub y} surface. Ex-situ contactmore » angle measurements show that SiN{sub x} and SiO{sub x}N{sub y} surfaces exposed to oxygen plasma are initially more hydrophilic than surfaces exposed to NH{sub 3} plasma, indicating that the O{sub 2} plasma-induced SiO{sub 2} overlayer is highly reactive toward ambient. At longer ambient exposures (≳10 h), however, surfaces treated by either O{sub 2} or NH{sub 3} plasma exhibit similar steady state contact angles, correlated with rapid uptake of adventitious carbon, as determined by XPS. Surface passivation by exposure to molecular hydrogen prior to ambient exposure significantly retards the increase in contact angle upon exposure to ambient. The results suggest a practical route to enhancing the time available for effective bonding to surfaces in microelectronics packaging applications.« less

Process for making boron nitride using sodium cyanide and boron

DOEpatents

Bamberger, Carlos E.

1990-02-06

This a very simple process for making boron nitride by mixing sodium cyanide and boron phosphate and heating the mixture in an inert atmosphere until a reaction takes place. The product is a white powder of boron nitride that can be used in applications that require compounds that are stable at high temperatures and that exhibit high electrical resistance.

Process for making boron nitride using sodium cyanide and boron

DOEpatents

Bamberger, Carlos E.

1990-01-01

This a very simple process for making boron nitride by mixing sodium cyanide and boron phosphate and heating the mixture in an inert atmosphere until a reaction takes place. The product is a white powder of boron nitride that can be used in applications that require compounds that are stable at high temperatures and that exhibit high electrical resistance.

Passivated niobium cavities

DOEpatents

Myneni, Ganapati Rao [Yorktown, VA; Hjorvarsson, Bjorgvin [Lagga Arby, SE; Ciovati, Gianluigi [Newport News, VA

2006-12-19

A niobium cavity exhibiting high quality factors at high gradients is provided by treating a niobium cavity through a process comprising: 1) removing surface oxides by plasma etching or a similar process; 2) removing hydrogen or other gases absorbed in the bulk niobium by high temperature treatment of the cavity under ultra high vacuum to achieve hydrogen outgassing; and 3) assuring the long term chemical stability of the niobium cavity by applying a passivating layer of a superconducting material having a superconducting transition temperature higher than niobium thereby reducing losses from electron (cooper pair) scattering in the near surface region of the interior of the niobium cavity. According to a preferred embodiment, the passivating layer comprises niobium nitride (NbN) applied by reactive sputtering.

Biofunctionalized silicon nitride platform for sensing applications.

PubMed

Hoi, Hiofan; Rezaie, Salva S; Gong, Lu; Sen, Payel; Zeng, Hongbo; Montemagno, Carlo; Gupta, Manisha

2018-04-15

Silicon nitride (SiN x ) based biosensors have the potential to converge on the technological achievements of semiconductor microfabrication and biotechnology. Development of biofunctionalized SiN x surface and its integration with other devices will allow us to integrate the biosensing capability with probe control, data acquisition and data processing. Here we use the hydrogen plasma generated by inductively coupled plasma-reactive ion etching (ICP-RIE) technique to produce amino-functionality on the surface of SiN x which can then be readily used for biomolecule immobilization. ICP-RIE produces high-density hydrogen ions/radicals at low energy, which produces high-density amino group on the SiN x surface within a short duration of time and with minimal surface damage. In this work, we have demonstrated selective amination of SiN x surface as compared to Si surface. The as-activated SiN x surface can be readily biofunctionalized with both protein and oligonucleotide through covalent immobilization. N-5-azido-2-nitrobenzoyloxysuccinimide, a photoactivable amino reactive bifunctional crosslinker, was used and greater than 90% surface coverage was achieved for protein immobilization. In addition, ssDNA immobilization and hybridization with its complemented strand was shown. Thus, we demonstrate a uniform, reliable, fast and economical technique for creating biofunctionalized SiN x surface that can be used for developing compact high-sensitivity biosensors. Copyright © 2017 Elsevier B.V. All rights reserved.

Materials Research Society Symposium Proceedings on Diamond, SiC and Nitride Wide Bandgap Semiconductors Held at San Francisco, California on 4-8 April 1994. Volume 339.

DTIC Science & Technology

1994-04-08

demonstrated that there existed no graphite phase at the surface of the as-deposited and 02 plasma treated polycrystalline diamond films. W 3- uO 2.5...diamond, highly ordered pyrolitic graphite ( HOPG ), and an amorphous carbon surface created by 1 keV ion bombardment of diamond. The diamond surface was...Library of Congress Cataloging in Publication Data Materials Research Society. Meeting (1994 : San Francisco, Calif.). Symposium D. Diamond, SiC and nitride

Application of low-temperature plasma for the synthesis of hydrogenated graphene (graphane)

NASA Astrophysics Data System (ADS)

Shavelkina, M. B.; Amirov, R. H.; Katarzhis, V. A.; Kiselev, V. I.

2017-12-01

The possibility of a direct synthesis of hydrogenated graphene in decomposition of methane by means of low-temperature plasma was investigated. A DC plasma torch with an expanding channel-anode, a vortex gas supply and a self-setting arc length was used as a generator of low-temperature plasma. Argon was used as the plasma-forming gas. The temperatures of argon plasma and with methane addition to it were determined on the basis of spectral measurements. The synthesis products were characterized by electron microscopy and thermogravimetry. The effect of hydrogenated graphene as a nanomodifier on the properties of the cubic boron nitride based functional ceramics was investigated.

Structure refinement for tantalum nitrides nanocrystals with various morphologies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Lianyun; School of Science, Beijing Jiaotong University, 3 Shang Yuan Cun, Haidian District, Beijing 100044; Huang, Kai

2012-07-15

Graphical abstract: Tantalum nitrides nanocrystals with various phases and morphologies for the first time have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. Highlights: ► The spherical TaN, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. ► The crystal structures of different tantalum nitrides were determined by Rietveld refinement on the X-ray diffraction data and the examinations of electron microcopies. ► The specific surface area of the tantalum nitrides powders was around 10 m{supmore » 2} g{sup −1}. ► Tantalum nitrides powders could be suitable for capacitor with high specific capacitance. -- Abstract: Tantalum nitrides (TaN{sub x}) nanocrystals with different phase and morphology have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. The crystal structures of tantalum nitrides were determined by Rietveld refinement based on the X-ray diffraction data. The morphologies of various tantalum nitrides nanocrystals in high quality were analyzed through the electron microcopies examinations. The spherical TaN nanoparticles, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been selectively prepared at different annealing temperatures. In addition, the specific surface areas of the tantalum nitrides nanocrystals measured by BET method were around 9.87–11.64 m{sup 2} g{sup −1}, indicating that such nano-sized tantalum nitrides could be suitable for capacitor with high specific capacitance.« less

Inverse magnetostrictive characteristics of Fe-Co composite materials using gas-nitriding process

NASA Astrophysics Data System (ADS)

Nakajima, Kenya; Yang, Zhenjun; Narita, Fumio

2018-03-01

The inverse magnetostrictive response, known as the Villari effect, of magnetostrictive materials is a change in magnetization due to an applied stress. It is commonly used for sensor applications. This work deals with the inverse magnetostrictive characteristics of Fe-Co bimetal plates that were subjected gas-nitriding process. Gas-nitriding was performed on bimetal plates for 30 min at 853 K as a surface heat treatment process. The specimens were cooled to room temperature after completing the nitriding treatment. Three-point bending tests were performed on the plates under a magnetic field. The changes on the magnetic induction of the plates due to the applied load are discussed. The effect of the nitriding treatment on the inverse magnetostrictive characteristics, magnetostrictive susceptibility, and magnetic hysteresis loop was examined. Our work represents an important step forward in the development of magnetostrictive sensor materials.

Dry etching, surface passivation and capping processes for antimonide based photodetectors

NASA Astrophysics Data System (ADS)

Dutta, Partha; Langer, Jeffery; Bhagwat, Vinay; Juneja, Jasbir

2005-05-01

III-V antimonide based devices suffer from leakage currents. Surface passivation and subsequent capping of the surfaces are absolutely essential for any practical applicability of antimonide based devices. The quest for a suitable surface passivation technology is still on. In this paper, we will present some of the promising recent developments in this area based on dry etching of GaSb based homojunction photodiodes structures followed by various passivation and capping schemes. We have developed a damage-free, universal dry etching recipe based on unique ratios of Cl2/BCl3/CH4/Ar/H2 in ECR plasma. This novel dry plasma process etches all III-V compounds at different rates with minimal damage to the side walls. In GaSb based photodiodes, an order of magnitude lower leakage current, improved ideality factor and higher responsivity has been demonstrated using this recipe compared to widely used Cl2/Ar and wet chemical etch recipes. The dynamic zero bias resistance-area product of the Cl2/BCl3/CH4/Ar/H2 etched diodes (830 Ω cm2) is higher than the Cl2/Ar (300 Ω cm2) and wet etched (330 Ω cm2) diodes. Ammonium sulfide has been known to passivate surfaces of III-V compounds. In GaSb photodiodes, the leakage current density reduces by a factor of 3 upon sulfur passivation using ammonium sulfide. However, device performance degrades over a period of time in the absence of any capping or protective layer. Silicon Nitride has been used as a cap layer by various researchers. We have found that by using silicon nitride caps, the devices exhibit higher leakage than unpassivated devices probably due to plasma damage during SiNx deposition. We have experimented with various polymers for capping material. It has been observed that ammonium sulfide passivation when combined with parylene capping layer (150 Å), devices retain their improved performance for over 4 months.

Improved growth of GaN layers on ultra thin silicon nitride/Si (1 1 1) by RF-MBE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Mahesh; Roul, Basanta; Central Research Laboratory, Bharat Electronics, Bangalore 560013

High-quality GaN epilayers were grown on Si (1 1 1) substrates by molecular beam epitaxy using a new growth process sequence which involved a substrate nitridation at low temperatures, annealing at high temperatures, followed by nitridation at high temperatures, deposition of a low-temperature buffer layer, and a high-temperature overgrowth. The material quality of the GaN films was also investigated as a function of nitridation time and temperature. Crystallinity and surface roughness of GaN was found to improve when the Si substrate was treated under the new growth process sequence. Micro-Raman and photoluminescence (PL) measurement results indicate that the GaN filmmore » grown by the new process sequence has less tensile stress and optically good. The surface and interface structures of an ultra thin silicon nitride film grown on the Si surface are investigated by core-level photoelectron spectroscopy and it clearly indicates that the quality of silicon nitride notably affects the properties of GaN growth.« less

Study on re-sputtering during CN{sub x} film deposition through spectroscopic diagnostics of plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, Peipei; Yang, Xu; Li, Hui

2015-10-15

A nitrogen-carbon plasma was generated during the deposition of carbon nitride (CN{sub x}) thin films by pulsed laser ablation of a graphite target in a discharge nitrogen plasma, and the optical emission of the generated nitrogen-carbon plasma was measured for the diagnostics of the plasma and the characterization of the process of CN{sub x} film deposition. The nitrogen-carbon plasma was recognized to contain various species including nitrogen molecules and molecular ions excited in the ambient N{sub 2} gas, carbon atoms and atomic ions ablated from the graphite target and CN radicals. The temporal evolution and spatial distribution of the CNmore » emission and their dependence on the substrate bias voltage show two groups of CN radicals flying in opposite directions. One represents the CN radicals formed as the products of the reactions occurring in the nitrogen-carbon plasma, revealing the reactive deposition of CN{sub x} film due to the reactive expansion of the ablation carbon plasma in the discharge nitrogen plasma and the effective formation of gaseous CN radicals as precursors for CN{sub x} film growth. The other one represents the CN radicals re-sputtered from the growing CN{sub x} film by energetic plasma species, evidencing the re-sputtering of the growing film accompanying film growth. And, the re-sputtering presents ion-induced sputtering features.« less

Physical fundamentals of criterial estimation of nitriding technology for parts of friction units

NASA Astrophysics Data System (ADS)

Kuksenova, L. I.; Gerasimov, S. A.; Lapteva, V. G.; Alekseeva, M. S.

2013-03-01

Characteristics of the structure and properties of surface layers of nitrided structural steels and alloys, which affect the level of surface fracture under friction, are studied. A generalized structural parameter for optimizing the nitriding process and a rapid method for estimating the quality of the surface layer of nitrided parts of friction units are developed.

Effect of MoO3 on the synthesis of boron nitride nanotubes over Fe and Ni catalysts.

PubMed

Nithya, Jeghan Shrine Maria; Pandurangan, Arumugam

2012-05-01

Synthesis of boron nitride nanotubes at reduced temperature is important for industrial manufactures. In this study boron nitride nanotubes were synthesized by thermal evaporation method using B/Fe2O3/MoO3 and B/Ni2O3/MoO3 mixtures separately with ammonia as the nitrogen source. The growth of boron nitride nanotubes occurred at 1100 degrees C, which was relatively lower than other metal oxides assisted growth processes requiring higher than 1200 degrees C. MoO3 promoted formation of B2O2 and aided boron nitride nanotubes growth at a reduced temperature. The boron nitride nanotubes with bamboo shaped, nested cone structured and straight tubes like forms were evident from the high resolution transmission electron microscopy. Metallic Fe and Ni, formed during the process, were the catalysts for the growth of boron nitride nanotubes. Their formation was established by X-ray diffraction. FT Raman showed a peak due to B-N vibration of BNNTs close to 1370 cm(-1). Hence MoO3 assisted growth of boron nitride nanotubes is advantageous, as it significantly reduced the synthesis temperature.

Application of hard coatings to substrates at low temperatures

NASA Technical Reports Server (NTRS)

Sproul, William D.

1993-01-01

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.

AlGaN Channel Transistors for Power Management and Distribution

NASA Technical Reports Server (NTRS)

VanHove, James M.

1996-01-01

Contained within is the Final report of a Phase 1 SBIR program to develop AlGaN channel junction field effect transistors (JFET). The report summarizes our work to design, deposit, and fabricate JFETS using molecular beam epitaxy growth AlGaN. Nitride growth is described using a RF atomic nitrogen plasma source. Processing steps needed to fabricate the device such as ohmic source-drain contacts, reactive ion etching, gate formation, and air bride fabrication are documented. SEM photographs of fabricated power FETS are shown. Recommendations are made to continue the effort in a Phase 2 Program.

Design, Control and in Situ Visualization of Gas Nitriding Processes

PubMed Central

Ratajski, Jerzy; Olik, Roman; Suszko, Tomasz; Dobrodziej, Jerzy; Michalski, Jerzy

2010-01-01

The article presents a complex system of design, in situ visualization and control of the commonly used surface treatment process: the gas nitriding process. In the computer design conception, analytical mathematical models and artificial intelligence methods were used. As a result, possibilities were obtained of the poly-optimization and poly-parametric simulations of the course of the process combined with a visualization of the value changes of the process parameters in the function of time, as well as possibilities to predict the properties of nitrided layers. For in situ visualization of the growth of the nitrided layer, computer procedures were developed which make use of the results of the correlations of direct and differential voltage and time runs of the process result sensor (magnetic sensor), with the proper layer growth stage. Computer procedures make it possible to combine, in the duration of the process, the registered voltage and time runs with the models of the process. PMID:22315536

Ion energy distributions in bipolar pulsed-dc discharges of methane measured at the biased cathode

NASA Astrophysics Data System (ADS)

Corbella, C.; Rubio-Roy, M.; Bertran, E.; Portal, S.; Pascual, E.; Polo, M. C.; Andújar, J. L.

2011-02-01

The ion fluxes and ion energy distributions (IED) corresponding to discharges in methane (CH4) were measured in time-averaged mode with a compact retarding field energy analyser (RFEA). The RFEA was placed on a biased electrode at room temperature, which was powered by either radiofrequency (13.56 MHz) or asymmetric bipolar pulsed-dc (250 kHz) signals. The shape of the resulting IED showed the relevant populations of ions bombarding the cathode at discharge parameters typical in the material processing technology: working pressures ranging from 1 to 10 Pa and cathode bias voltages between 100 and 200 V. High-energy peaks in the IED were detected at low pressures, whereas low-energy populations became progressively dominant at higher pressures. This effect is attributed to the transition from collisionless to collisional regimes of the cathode sheath as the pressure increases. On the other hand, pulsed-dc plasmas showed broader IED than RF discharges. This fact is connected to the different working frequencies and the intense peak voltages (up to 450 V) driven by the pulsed power supply. This work improves our understanding in plasma processes at the cathode level, which are of crucial importance for the growth and processing of materials requiring controlled ion bombardment. Examples of industrial applications with these requirements are plasma cleaning, ion etching processes during fabrication of microelectronic devices and plasma-enhanced chemical vapour deposition of hard coatings (diamond-like carbon, carbides and nitrides).

Thermal Improvement and Stability of Si3N4/GeNx/p- and n-Ge Structures Prepared by Electron-Cyclotron-Resonance Plasma Nitridation and Sputtering at Room Temperature

NASA Astrophysics Data System (ADS)

Fukuda, Yukio; Okamoto, Hiroshi; Iwasaki, Takuro; Izumi, Kohei; Otani, Yohei; Ishizaki, Hiroki; Ono, Toshiro

2012-09-01

This paper reports on the thermal improvement of Si3N4/GeNx/Ge structures. After the Si3N4 (5 nm)/GeNx (2 nm) stacks were prepared on Ge substrates by electron-cyclotron-resonance plasma nitridation and sputtering at room temperature, they were thermally annealed in atmospheric N2 + 10% H2 ambient at temperatures from 400 to 600 °C. It was demonstrated that the electronic properties of the GeNx/Ge interfaces were thermally improved at temperatures of up to 500 °C with a minimum interface trap density (Dit) of ˜1×1011 cm-2 eV-1 near the Ge midgap, whereas the interface properties were slightly degraded after annealing at 600 °C with a minimum Dit value of ˜4×1011 cm-2 eV-1.

Cathodic cage plasma deposition of TiN and TiO{sub 2} thin films on silicon substrates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sousa, Romulo R. M. de; Sato, Patricia S.; Nascente, Pedro A. P., E-mail: nascente@ufscar.br

2015-07-15

Cathodic cage plasma deposition (CCPD) was used for growing titanium nitride (TiN) and titanium dioxide (TiO{sub 2}) thin films on silicon substrates. The main advantages of the CCPD technique are the uniformity, tridimensionality, and high rate of the film deposition that occurs at higher pressures, lower temperatures, and lower treatment times than those used in conventional nitriding treatments. In this work, the influence of the temperature and gas atmosphere upon the characteristics of the deposited films was investigated. The TiN and TiO{sub 2} thin films were characterized by x-ray diffraction, scanning electron microscopy, and Raman spectroscopy to analyze their chemical,more » structural, and morphological characteristics, and the combination of these results indicates that the low-cost CCPD technique can be used to produce even and highly crystalline TiN and TiO{sub 2} films.« less

Study of the wear resistance of ion-plasma coatings based on titanium and aluminum and obtained by magnetron sputtering

NASA Astrophysics Data System (ADS)

Kachalin, G. V.; Mednikov, A. F.; Tkhabisimov, A. B.; Sidorov, S. V.

2017-05-01

The paper presents the results of metallographic researches and erosion tests of ion-plasma coatings (based on titanium, aluminum and their nitrides), which were formed on samples of 12Kh13 and EI961 blade steels. Erosion tests and studies of characteristics of obtained by magnetron sputtering coatings were carried out by using a set of research equipment UNU “Erosion-M” NRU “MPEI”. It was found that the formed Ti/Al-TiN/AlN coatings increase the duration of blade steels erosion wear incubation period by at least in 1.5 times and have a layered structure with thicknesses of nitride layers 1.3-1.6 μm and intermediate metallic layers 0.3-0.5 μm, with a total thickness of coatings of 10-14 μm for 12Kh13steel samples and 19-21 μm for EI961 steel samples.

Laser Plasma Soft X-ray Microscope with Wolter Mirrors for Observation of Biological Specimens in Air

NASA Astrophysics Data System (ADS)

Hoshino, Masato; Aoki, Sadao

2006-02-01

A laser plasma soft X-ray microscope with Wolter mirrors was developed so that specimens could be set in the atmosphere. Silicon nitride membranes 100 nm thick were used as vacuum-tight windows. Using relatively large windows (0.46× 0.46 mm2), an adequate working distance for samples, which was approximately 1.2 mm, was assured. The endurance of the vacuum-tight window was measured briefly. Dry biological cells could be observed with resolution better than 100 nm. A preliminary observation of wet biological cells was carried out using a wet environmental sample holder which was composed of only two sheets of silicon nitride membrane. An X-ray micrograph of wet red blood cells from a chicken was obtained without apparent effects of radiation damage. The properties of a vacuum-tight window and a wet sample holder are discussed.

Control of the Structure of Diffusion Layer in Carbon Steels Under Nitriding with Preliminary Deposition of Copper Oxide Catalytic Films

NASA Astrophysics Data System (ADS)

Petrova, L. G.; Aleksandrov, V. A.; Malakhov, A. Yu.

2017-07-01

The effect of thin films of copper oxide deposited before nitriding on the phase composition and the kinetics of growth of diffusion layers in carbon steels is considered. The process of formation of an oxide film involves chemical reduction of pure copper on the surface of steel specimens from a salt solution and subsequent oxidation under air heating. The oxide film exerts a catalytic action in nitriding of low- and medium-carbon steels, which consists in accelerated growth of the diffusion layer, the nitride zone in the first turn. The kinetics of the nitriding process and the phase composition of the layer are controlled by the thickness of the copper oxide precursor, i.e., the deposited copper film.

Silicon nitride films fabricated by a plasma-enhanced chemical vapor deposition method for coatings of the laser interferometer gravitational wave detector

NASA Astrophysics Data System (ADS)

Pan, Huang-Wei; Kuo, Ling-Chi; Huang, Shu-Yu; Wu, Meng-Yun; Juang, Yu-Hang; Lee, Chia-Wei; Chen, Hsin-Chieh; Wen, Ting Ting; Chao, Shiuh

2018-01-01

Silicon is a potential substrate material for the large-areal-size mirrors of the next-generation laser interferometer gravitational wave detector operated in cryogenics. Silicon nitride thin films uniformly deposited by a chemical vapor deposition method on large-size silicon wafers is a common practice in the silicon integrated circuit industry. We used plasma-enhanced chemical vapor deposition to deposit silicon nitride films on silicon and studied the physical properties of the films that are pertinent to application of mirror coatings for laser interferometer gravitational wave detectors. We measured and analyzed the structure, optical properties, stress, Young's modulus, and mechanical loss of the films, at both room and cryogenic temperatures. Optical extinction coefficients of the films were in the 10-5 range at 1550-nm wavelength. Room-temperature mechanical loss of the films varied in the range from low 10-4 to low 10-5 within the frequency range of interest. The existence of a cryogenic mechanical loss peak depended on the composition of the films. We measured the bond concentrations of N - H , Si - H , Si - N , and Si - Si bonds in the films and analyzed the correlations between bond concentrations and cryogenic mechanical losses. We proposed three possible two-level systems associated with the N - H , Si - H , and Si - N bonds in the film. We inferred that the dominant source of the cryogenic mechanical loss for the silicon nitride films is the two-level system of exchanging position between a H+ and electron lone pair associated with the N - H bond. Under our deposition conditions, superior properties in terms of high refractive index with a large adjustable range, low optical absorption, and low mechanical loss were achieved for films with lower nitrogen content and lower N - H bond concentration. Possible pairing of the silicon nitride films with other materials in the quarter-wave stack is discussed.

Effect of processing parameters on reaction bonding of silicon nitride

NASA Technical Reports Server (NTRS)

Richman, M. H.; Gregory, O. J.; Magida, M. B.

1980-01-01

Reaction bonded silicon nitride was developed. The relationship between the various processing parameters and the resulting microstructures was to design and synthesize reaction bonded materials with improved room temperature mechanical properties.

Ion-induced crystal damage during plasma-assisted MBE growth of GaN layers

NASA Astrophysics Data System (ADS)

Kirchner, V.; Heinke, H.; Birkle, U.; Einfeldt, S.; Hommel, D.; Selke, H.; Ryder, P. L.

1998-12-01

Gallium nitride layers were grown by plasma-assisted molecular-beam epitaxy on (0001)-oriented sapphire substrates using an electron cyclotron resonance (ECR) and a radio frequency (rf) plasma source. An applied substrate bias was varied from -200 to +250 V, resulting in a change of the density and energy of nitrogen ions impinging the growth surface. The layers were investigated by high-resolution x-ray diffractometry and high-resolution transmission electron microscopy (HRTEM). Applying a negative bias during growth has a marked detrimental effect on the crystal perfection of the layers grown with an ECR plasma source. This is indicated by a change in shape and width of (0002) and (202¯5) reciprocal lattice points as monitored by triple axis x-ray measurements. In HRTEM images, isolated basal plane stacking faults were found, which probably result from precipitation of interstitial atoms. The crystal damage in layers grown with a highly negative substrate bias is comparable to that observed for ion implantation processes at orders of magnitude larger ion energies. This is attributed to the impact of ions on the growing surface. None of the described phenomena was observed for the samples grown with the rf plasma source.

In vitro corrosion resistance of plasma source ion nitrided austenitic stainless steels.

PubMed

Le, M K; Zhu, X M

2001-04-01

Plasma source ion nitriding has emerged as a low-temperature, low-pressure nitriding approach for low-energy implanting nitrogen ions and then diffusing them into steel and alloy. In this work, a single high nitrogen face-centered-cubic (f.c.c.) phase (gammaN) formed on the 1Cr18Ni9Ti and AISI 316L austenitic stainless steels with a high nitrogen concentration of about 32 at % was characterized using Auger electron spectroscopy, electron probe microanalysis, glancing angle X-ray diffraction, and transmission electron microscopy. The corrosion resistance of the gammaN-phase layer was studied by the electrochemical cyclic polarization measurement in Ringer's solutions buffered to pH from 3.5 to 7.2 at a temperature of 37 degrees C. No pitting corrosion in the Ringer's solutions with pH = 7.2 and 5.5 was detected for the gammaN-phase layers on the two stainless steels. The high pitting potential for the gammaN-phase layers is higher, about 500 and 600 mV, above that of the two original stainless steels, respectively, in the Ringer's solution with pH = 3.5. The corroded surface morphologies of the gammaN-phase layers observed by scanning electron microscopy are consistent with the results of the electrochemical polarization measurement.

Heuristic Analysis Model of Nitrided Layers’ Formation Consisting of the Image Processing and Analysis and Elements of Artificial Intelligence

PubMed Central

Wójcicki, Tomasz; Nowicki, Michał

2016-01-01

The article presents a selected area of research and development concerning the methods of material analysis based on the automatic image recognition of the investigated metallographic sections. The objectives of the analyses of the materials for gas nitriding technology are described. The methods of the preparation of nitrided layers, the steps of the process and the construction and operation of devices for gas nitriding are given. We discuss the possibility of using the methods of digital images processing in the analysis of the materials, as well as their essential task groups: improving the quality of the images, segmentation, morphological transformations and image recognition. The developed analysis model of the nitrided layers formation, covering image processing and analysis techniques, as well as selected methods of artificial intelligence are presented. The model is divided into stages, which are formalized in order to better reproduce their actions. The validation of the presented method is performed. The advantages and limitations of the developed solution, as well as the possibilities of its practical use, are listed. PMID:28773389

Effects of Temperature on Microstructure and Wear of Salt Bath Nitrided 17-4PH Stainless Steel

NASA Astrophysics Data System (ADS)

Wang, Jun; Lin, Yuanhua; Fan, Hongyuan; Zeng, Dezhi; Peng, Qian; Shen, Baoluo

2012-08-01

Salt bath nitriding of 17-4 PH martensitic precipitation hardening stainless steels was conducted at 610, 630, and 650 °C for 2 h using a complex salt bath heat-treatment, and the properties of the nitrided surface were systematically evaluated. Experimental results revealed that the microstructure and phase constituents of the nitrided surface alloy are highly process condition dependent. When 17-4PH stainless steel was subjected to complex salt bathing nitriding, the main phase of the nitrided layer was expanded martensite (α'), expanded austenite (γN), CrN, Fe4N, and (Fe,Cr) x O y . In the sample nitrided above 610 °C, the expanded martensite transformed into expanded austenite. But in the sample nitrided at 650 °C, the expanded austenite decomposed into αN and CrN. The decomposed αN then disassembled into CrN and alpha again. The nitrided layer depth thickened intensively with the increasing nitriding temperature. The activation energy of nitriding in this salt bath was 125 ± 5 kJ/mol.

Water treatment by the AC gliding arc air plasma

NASA Astrophysics Data System (ADS)

Gharagozalian, Mehrnaz; Dorranian, Davoud; Ghoranneviss, Mahmood

2017-09-01

In this study, the effects of gliding arc (G Arc) plasma system on the treatment of water have been investigated experimentally. An AC power supply of 15 kV potential difference at 50 Hz frequency was employed to generate plasma. Plasma density and temperature were measured using spectroscopic method. The water was contaminated with staphylococcus aureus (Gram-positive) and salmonella bacteria (Gram-negative), and Penicillium (mold fungus) individually. pH, hydrogen peroxide, and nitride contents of treated water were measured after plasma treatment. Decontamination of treated water was determined using colony counting method. Results indicate that G Arc plasma is a powerful and green tool to decontaminate water without producing any byproducts.

Improved reaction sintered silicon nitride. [protective coatings to improve oxidation resistance

NASA Technical Reports Server (NTRS)

Baumgartner, H. R.

1978-01-01

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.

Formation of porous surface layers in reaction bonded silicon nitride during processing

NASA Technical Reports Server (NTRS)

Shaw, N. J.; Glasgow, T. K.

1979-01-01

An effort was undertaken to determine if the formation of the generally observed layer of large porosity adjacent to the as-nitride surfaces of reaction bonded silicon nitrides could be prevented during processing. Isostatically pressed test bars were prepared from wet vibratory milled Si powder. Sintering and nitriding were each done under three different conditions:(1) bars directly exposed to the furnance atmosphere; (2) bars packed in Si powder; (3) bars packed in Si3N4 powder. Packing the bars in either Si of Si3N4 powder during sintering retarded formation of the layer of large porosity. Only packing the bars in Si prevented formation of the layer during nitridation. The strongest bars (316 MPa) were those sintered in Si and nitrided in Si3N4 despite their having a layer of large surface porosity; failure initiated at very large pores and inclusions. The alpha/beta ratio was found to be directly proportional to the oxygen content; a possible explanation for this relationship is discussed.

The adhesion solidity, physico-mechanical and tribological properties of the coating of titanium nitride

NASA Astrophysics Data System (ADS)

Krivina, L. A.; Tarasenko, Yu P.; Fel, Ya A.

2017-05-01

Influence of variable technological factors (arch current, fractional pressure of gas in the camera) on structure, physic-mechanical and tribological features of an ion-plasma coating of titanium nitride has been investigated. The adhesion solidity has been put to the test and the mechanism of destruction of a covering has been also researched by a skretch-test method. The optimal mode of spraying at which the formation of the nanostructured bar coating of TiN has been defined. The covering offers an optimal combination of physic-mechanical, tribological and solidity features.

Electrochemical Solution Growth of Magnetic Nitrides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Monson, Todd C.; Pearce, Charles

Magnetic nitrides, if manufactured in bulk form, would provide designers of transformers and inductors with a new class of better performing and affordable soft magnetic materials. According to experimental results from thin films and/or theoretical calculations, magnetic nitrides would have magnetic moments well in excess of current state of the art soft magnets. Furthermore, magnetic nitrides would have higher resistivities than current transformer core materials and therefore not require the use of laminates of inactive material to limit eddy current losses. However, almost all of the magnetic nitrides have been elusive except in difficult to reproduce thin films or asmore » inclusions in another material. Now, through its ability to reduce atmospheric nitrogen, the electrochemical solution growth (ESG) technique can bring highly sought after (and previously inaccessible) new magnetic nitrides into existence in bulk form. This method utilizes a molten salt as a solvent to solubilize metal cations and nitrogen ions produced electrochemically and form nitrogen compounds. Unlike other growth methods, the scalable ESG process can sustain high growth rates (~mm/hr) even under reasonable operating conditions (atmospheric pressure and 500 °C). Ultimately, this translates into a high throughput, low cost, manufacturing process. The ESG process has already been used successfully to grow high quality GaN. Below, the experimental results of an exploratory express LDRD project to access the viability of the ESG technique to grow magnetic nitrides will be presented.« less

Stress evolution of Ge nanocrystals in dielectric matrices.

PubMed

Bahariqushchi, Rahim; Raciti, Rosario; Kasapoğlu, Ahmet Emre; Gür, Emre; Sezen, Meltem; Kalay, Eren; Mirabella, Salvatore; Aydinli, A

2018-05-04

Germanium nanocrystals (Ge NCs) embedded in single and multilayer silicon oxide and silicon nitride matrices have been synthesized using plasma enhanced chemical vapor deposition followed by conventional furnace annealing or rapid thermal processing in N 2 ambient. Compositions of the films were determined by Rutherford backscattering spectrometry and x-ray photoelectron spectroscopy. The formation of NCs under suitable process conditions was observed with high resolution transmission electron microscope micrographs and Raman spectroscopy. Stress measurements were done using Raman shifts of the Ge optical phonon line at 300.7 cm -1 . The effect of the embedding matrix and annealing methods on Ge NC formation were investigated. In addition to Ge NCs in single layer samples, the stress on Ge NCs in multilayer samples was also analyzed. Multilayers of Ge NCs in a silicon nitride matrix separated by dielectric buffer layers to control the size and density of NCs were fabricated. Multilayers consisted of SiN y :Ge ultrathin films sandwiched between either SiO 2 or Si 3 N 4 by the proper choice of buffer material. We demonstrated that it is possible to tune the stress state of Ge NCs from compressive to tensile, a desirable property for optoelectronic applications. We also observed that there is a correlation between the stress and the crystallization threshold in which the compressive stress enhances the crystallization, while the tensile stress suppresses the process.

Stress evolution of Ge nanocrystals in dielectric matrices

NASA Astrophysics Data System (ADS)

Bahariqushchi, Rahim; Raciti, Rosario; Emre Kasapoğlu, Ahmet; Gür, Emre; Sezen, Meltem; Kalay, Eren; Mirabella, Salvatore; Aydinli, A.

2018-05-01

Germanium nanocrystals (Ge NCs) embedded in single and multilayer silicon oxide and silicon nitride matrices have been synthesized using plasma enhanced chemical vapor deposition followed by conventional furnace annealing or rapid thermal processing in N2 ambient. Compositions of the films were determined by Rutherford backscattering spectrometry and x-ray photoelectron spectroscopy. The formation of NCs under suitable process conditions was observed with high resolution transmission electron microscope micrographs and Raman spectroscopy. Stress measurements were done using Raman shifts of the Ge optical phonon line at 300.7 cm-1. The effect of the embedding matrix and annealing methods on Ge NC formation were investigated. In addition to Ge NCs in single layer samples, the stress on Ge NCs in multilayer samples was also analyzed. Multilayers of Ge NCs in a silicon nitride matrix separated by dielectric buffer layers to control the size and density of NCs were fabricated. Multilayers consisted of SiN y :Ge ultrathin films sandwiched between either SiO2 or Si3N4 by the proper choice of buffer material. We demonstrated that it is possible to tune the stress state of Ge NCs from compressive to tensile, a desirable property for optoelectronic applications. We also observed that there is a correlation between the stress and the crystallization threshold in which the compressive stress enhances the crystallization, while the tensile stress suppresses the process.

The role of nano-particles in the field of thermal spray coating technology

NASA Astrophysics Data System (ADS)

Siegmann, Stephan; Leparoux, Marc; Rohr, Lukas

2005-06-01

Nano-particles play not only a key role in recent research fields, but also in the public discussions about health and safety in nanotechnology. Nevertheless, the worldwide activities in nano-particles research increased dramatically during the last 5 to 10 years. There are different potential routes for the future production of nano-particles at large scale. The main directions envisaged are mechanical milling, wet chemical reactions or gas phase processes. Each of the processes has its specific advantages and limitations. Mechanical milling and wet chemical reactions are typically time intensive and batch processes, whereas gas phase productions by flames or plasma can be carried out continuously. Materials of interest are mainly oxide ceramics, carbides, nitrides, and pure metals. Nano-ceramics are interesting candidates for coating technologies due to expected higher coating toughness, better thermal shock and wear resistance. Especially embedded nano-carbides and-nitrides offer homogenously distributed hard phases, which enhance coatings hardness. Thermal spraying, a nearly 100 years old and world wide established coating technology, gets new possibilities thanks to optimized, nano-sized and/or nano-structured powders. Latest coating system developments like high velocity flame spraying (HVOF), cold gas deposition or liquid suspension spraying in combination with new powder qualities may open new applications and markets. This article gives an overview on the latest activities in nano-particle research and production in special relation to thermal spray coating technology.

Exploring electrolyte preference of vanadium nitride supercapacitor electrodes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Bo; Chen, Zhaohui; Lu, Gang

Highlights: • Hierarchical VN nanostructures were prepared on graphite foam. • Electrolyte preference of VN supercapacitor electrodes was explored. • VN showed better capacitive property in organic and alkaline electrolytes than LiCl. - Abstract: Vanadium nitride hierarchical nanostructures were prepared through an ammonia annealing procedure utilizing vanadium pentoxide nanostructures grown on graphite foam. The electrochemical properties of hierarchical vanadium nitride was tested in aqueous and organic electrolytes. As a result, the vanadium nitride showed better capacitive energy storage property in organic and alkaline electrolytes. This work provides insight into the charge storage process of vanadium nitride and our findings canmore » shed light on other transition metal nitride-based electrochemical energy storage systems.« less

Cubic nitride templates

DOEpatents

Burrell, Anthony K; McCleskey, Thomas Mark; Jia, Quanxi; Mueller, Alexander H; Luo, Hongmei

2013-04-30

A polymer-assisted deposition process for deposition of epitaxial cubic metal nitride films and the like is presented. The process includes solutions of one or more metal precursor and soluble polymers having binding properties for the one or more metal precursor. After a coating operation, the resultant coating is heated at high temperatures under a suitable atmosphere to yield metal nitride films and the like. Such films can be used as templates for the development of high quality cubic GaN based electronic devices.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Malik, Hitendra K., E-mail: hkmalik@physics.iitd.ac.in; Singh, Omveer; Dahiya, Raj P.

We have established a hot cathode arc discharge plasma system, where different stainless steel samples can be treated by monitoring the plasma parameters and nitriding parameters independently. In the present work, a mixture of 70% N{sub 2} and 30% H{sub 2} gases was fed into the plasma chamber and the treatment time and substrate temperature were optimized for treating 304L Stainless Steel samples. Various physical techniques such as x-ray diffraction, energy dispersive x-ray spectroscopy and micro-vickers hardness tester were employed to determine the structural, surface composition and surface hardness of the treated samples.

Cavitation Erosion in Hydraulic Turbine Components and Mitigation by Coatings: Current Status and Future Needs

NASA Astrophysics Data System (ADS)

Singh, Raghuvir; Tiwari, S. K.; Mishra, Suman K.

2012-07-01

Cavitation erosion is a frequently observed phenomenon in underwater engineering materials and is the primary reason for component failure. The damage due to cavitation erosion is not yet fully understood, as it is influenced by several parameters, such as hydrodynamics, component design, environment, and material chemistry. This article gives an overview of the current state of understanding of cavitation erosion of materials used in hydroturbines, coatings and coating methodologies for combating cavitation erosion, and methods to characterize cavitation erosion. No single material property fully characterizes the resistance to cavitation erosion. The combination of ultimate resilience, hardness, and toughness rather may be useful to estimate the cavitation erosion resistance of material. Improved hydrodynamic design and appropriate surface engineering practices reduce damage due to cavitation erosion. The coatings suggested for combating the cavitation erosion encompasses carbides (WC Cr2C3, Cr3C2, 20CrC-80WC), cermets of different compositions (e.g., 56W2C/Ni/Cr, 41WC/Ni/Cr/Co), intermetallic composites, intermetallic matrix composites with TiC reinforcement, composite nitrides such as TiAlN and elastomers. A few of them have also been used commercially. Thermal spraying, arc plasma spraying, and high velocity oxy-fuel (HVOF) processes have been used commercially to apply the coatings. Boronizing, laser surface hardening and cladding, chemical vapor deposition, physical vapor deposition, and plasma nitriding have been tried for surface treatments at laboratory levels and have shown promise to be used on actual components.

Hollow Cathode Plasma-Enhanced Atomic Layer Deposition of Silicon Nitride Using Pentachlorodisilane.

PubMed

Meng, Xin; Kim, Harrison Sejoon; Lucero, Antonio T; Hwang, Su Min; Lee, Joy S; Byun, Young-Chul; Kim, Jiyoung; Hwang, Byung Keun; Zhou, Xiaobing; Young, Jeanette; Telgenhoff, Michael

2018-04-25

In this work, a novel chlorodisilane precursor, pentachlorodisilane (PCDS, HSi 2 Cl 5 ), was investigated for the growth of silicon nitride (SiN x ) via hollow cathode plasma-enhanced atomic layer deposition (PEALD). A well-defined self-limiting growth behavior was successfully demonstrated over the growth temperature range of 270-360 °C. At identical process conditions, PCDS not only demonstrated approximately >20% higher growth per cycle than that of a commercially available chlorodisilane precursor, hexachlorodisilane (Si 2 Cl 6 ), but also delivered a better or at least comparable film quality determined by characterizing the refractive index, wet etch rate, and density of the films. The composition of the SiN x films grown at 360 °C using PCDS, as determined by X-ray photoelectron spectroscopy, showed low O content (∼2 at. %) and Cl content (<1 at. %; below the detection limit). Fourier transform infrared spectroscopy spectra suggested that N-H bonds were the dominant hydrogen-containing bonds in the SiN x films without a significant amount of Si-H bonds originating from the precursor molecules. The possible surface reaction pathways of the PEALD SiN x using PCDS on the surface terminated with amine groups (-NH 2 and -NH-) are proposed. The PEALD SiN x films grown using PCDS also exhibited a leakage current density as low as 1-2 nA/cm 2 at 2 MV/cm and a breakdown electric field as high as ∼12 MV/cm.

Nitride coating enhances endothelialization on biomedical NiTi shape memory alloy.

PubMed

Ion, Raluca; Luculescu, Catalin; Cimpean, Anisoara; Marx, Philippe; Gordin, Doina-Margareta; Gloriant, Thierry

2016-05-01

Surface nitriding was demonstrated to be an effective process for improving the biocompatibility of implantable devices. In this study, we investigated the benefits of nitriding the NiTi shape memory alloy for vascular stent applications. Results from cell experiments indicated that, compared to untreated NiTi, a superficial gas nitriding treatment enhanced the adhesion of human umbilical vein endothelial cells (HUVECs), cell spreading and proliferation. This investigation provides data to demonstrate the possibility of improving the rate of endothelialization on NiTi by means of nitride coating. Copyright © 2016 Elsevier B.V. All rights reserved.

Process for preparing transition metal nitrides and transition metal carbonitrides and their reaction intermediates

DOEpatents

Maya, Leon

1988-05-24

A process for making ammonolytic precursors to nitride and carbonitride ceramics. Extreme reaction conditions are not required and the precursor is a powder-like substance that produces ceramics of improved purity and morphology upon pyrolysis.

Processing study of injection molding of silicon nitride for engine applications

NASA Technical Reports Server (NTRS)

Rorabaugh, M. E.; Yeh, H. C.

1985-01-01

The high hardness of silicon nitride, which is currently under consideration as a structural material for such hot engine components as turbine blades, renders machining of the material prohibitively costly; the near net shape forming technique of injection molding is accordingly favored as a means for component fabrication. Attention is presently given to the relationships between injection molding processing parameters and the resulting microstructural and mechanical properties of the resulting engine parts. An experimental program has been conducted under NASA sponsorship which tests the quality of injection molded bars of silicon nitride at various stages of processing.

Alkaline fuel cell with nitride membrane

NASA Astrophysics Data System (ADS)

Sun, Shen-Huei; Pilaski, Moritz; Wartmann, Jens; Letzkus, Florian; Funke, Benedikt; Dura, Georg; Heinzel, Angelika

2017-06-01

The aim of this work is to fabricate patterned nitride membranes with Si-MEMS-technology as a platform to build up new membrane-electrode-assemblies (MEA) for alkaline fuel cell applications. Two 6-inch wafer processes based on chemical vapor deposition (CVD) were developed for the fabrication of separated nitride membranes with a nitride thickness up to 1 μm. The mechanical stability of the perforated nitride membrane has been adjusted in both processes either by embedding of subsequent ion implantation step or by optimizing the deposition process parameters. A nearly 100% yield of separated membranes of each deposition process was achieved with layer thickness from 150 nm to 1 μm and micro-channel pattern width of 1μm at a pitch of 3 μm. The process for membrane coating with electrolyte materials could be verified to build up MEA. Uniform membrane coating with channel filling was achieved after the optimization of speed controlled dip-coating method and the selection of dimethylsulfoxide (DMSO) as electrolyte solvent. Finally, silver as conductive material was defined for printing a conductive layer onto the MEA by Ink-Technology. With the established IR-thermography setup, characterizations of MEAs in terms of catalytic conversion were performed successfully. The results of this work show promise for build up a platform on wafer-level for high throughput experiments.

Silicon Nitride Photonic Integration Platforms for Visible, Near-Infrared and Mid-Infrared Applications

PubMed Central

Micó, Gloria; Pastor, Daniel; Pérez, Daniel; Doménech, José David; Fernández, Juan; Baños, Rocío; Alemany, Rubén; Sánchez, Ana M.; Cirera, Josep M.; Mas, Roser

2017-01-01

Silicon nitride photonics is on the rise owing to the broadband nature of the material, allowing applications of biophotonics, tele/datacom, optical signal processing and sensing, from visible, through near to mid-infrared wavelengths. In this paper, a review of the state of the art of silicon nitride strip waveguide platforms is provided, alongside the experimental results on the development of a versatile 300 nm guiding film height silicon nitride platform. PMID:28895906

Boron Nitride Nanoribbons from Exfoliation of Boron Nitride Nanotubes

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh; Hurst, Janet; Santiago, Diana

2017-01-01

Two types of boron nitride nanotubes (BNNTs) were exfoliated into boron nitride nanoribbons (BNNR), which were identified using transmission electron microscopy: (1) commercial BNNTs with thin tube walls and small diameters. Tube unzipping was indicated by a large decrease of the sample's surface area and volume for pores less than 2 nm in diameter. (2) BNNTs with large diameters and thick walls synthesized at NASA Glenn Research Center. Here, tube unraveling was indicated by a large increase in external surface area and pore volume. For both, the exfoliation process was similar to the previous reported method to exfoliate commercial hexagonal boron nitride (hBN): Mixtures of BNNT, FeCl3, and NaF (or KF) were sequentially treated in 250 to 350 C nitrogen for intercalation, 500 to 750 C air for exfoliation, and finally HCl for purification. Property changes of the nanosized boron nitride throughout this process were also similar to the previously observed changes of commercial hBN during the exfoliation process: Both crystal structure (x-ray diffraction data) and chemical properties (Fourier-transform infrared spectroscopy data) of the original reactant changed after intercalation and exfoliation, but most (not all) of these changes revert back to those of the reactant once the final, purified products are obtained.

Process for producing silicon nitride based articles of high fracture toughness and strength

DOEpatents

Huckabee, Marvin; Buljan, Sergej-Tomislav; Neil, Jeffrey T.

1991-01-01

A process for producing a silicon nitride-based article of improved fracture toughness and strength. The process involves densifying to at least 98% of theoretical density a mixture including (a) a bimodal silicon nitride powder blend consisting essentially of about 10-30% by weight of a first silicon nitride powder of an average particle size of about 0.2 .mu.m and a surface area of about 8-12 m.sup.2 /g, and about 70-90% by weight of a second silicon nitride powder of an average particle size of about 0.4-0.6 .mu.m and a surface area of about 2-4 m.sup.2 /g, (b) about 10-50 percent by volume, based on the volume of the densified article, of refractory whiskers or fibers having an aspect ratio of about 3-150 and having an equivalent diameter selected to produce in the densified article an equivalent diameter ratio of the whiskers or fibers to grains of silicon nitride of greater than 1.0, and (c) an effective amount of a suitable oxide densification aid. Optionally, the mixture may be blended with a binder and injection molded to form a green body, which then may be densified by, for example, hot isostatic pressing.

Process for producing silicon nitride based articles of high fracture toughness and strength

DOEpatents

Huckabee, M.; Buljan, S.T.; Neil, J.T.

1991-09-10

A process for producing a silicon nitride-based article of improved fracture toughness and strength is disclosed. The process involves densifying to at least 98% of theoretical density a mixture including (a) a bimodal silicon nitride powder blend consisting essentially of about 10-30% by weight of a first silicon nitride powder of an average particle size of about 0.2 [mu]m and a surface area of about 8-12 m[sup 2]/g, and about 70-90% by weight of a second silicon nitride powder of an average particle size of about 0.4-0.6 [mu]m and a surface area of about 2-4 m[sup 2]/g, (b) about 10-50 percent by volume, based on the volume of the densified article, of refractory whiskers or fibers having an aspect ratio of about 3-150 and having an equivalent diameter selected to produce in the densified article an equivalent diameter ratio of the whiskers or fibers to grains of silicon nitride of greater than 1.0, and (c) an effective amount of a suitable oxide densification aid. Optionally, the mixture may be blended with a binder and injection molded to form a green body, which then may be densified by, for example, hot isostatic pressing.

A novel anti-frictional multiphase layer produced by plasma nitriding of PVD titanium coated ZL205A aluminum alloy

NASA Astrophysics Data System (ADS)

Lu, C.; Yao, J. W.; Wang, Y. X.; Zhu, Y. D.; Guo, J. H.; Wang, Y.; Fu, H. Y.; Chen, Z. B.; Yan, M. F.

2018-02-01

The heat treatment (consisting of solid solution and aging), is integrated with the nitriding process of titanium coated ZL205A aluminum alloy to improve the surface and matrix mechanical properties simultaneously. Two-step duplex treatment is adopted to prepare the gradient multiphase layer on a magnesium-free ZL205A aluminum-copper based alloy. Firstly, pure titanium film is deposited on the aluminum alloy substrate using magnetron sputtering. Secondly, the Ti-coated specimen is nitrided at the solid solution temperature of the substrate alloying elements in a gas mixture of N2 and H2 and aged at 175 °C. The microstructure evolution, microhardness as well as the wear resistance of obtained multiphase layers are investigated by means of scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), microhardness tester and pin-on-disc tribometer. The multiphase layer, dominated by TiN0.3 or Al3Ti, is prepared with significantly increased layer depth after duplex treatment. The surface hardness of multiphase layer is remarkably improved from 23.7HV to 457HV. The core matrix hardness is also increased to 65HV after aging. The wear rate of the multiphase layer decreases about 55.22% and 49.28% in comparison with the aged and Ti coated specimens, respectively. The predominant wear mechanism for the multiphase layer is abrasive and oxidation, but severe adhesive wear for the aged and Ti coated specimens.

TEM studies of plasma nitrided austenitic stainless steel.

PubMed

Stróz, D; Psoda, M

2010-03-01

Cross-sectional transmission electron microscopy and X-ray phase analysis were used to study the structure of a layer formed during nitriding the AISI 316L stainless steel at temperature 440 degrees C. It was found that the applied treatment led to the formation of 6-microm-thick layer of the S-phase. There is no evidence of CrN precipitation. The X-ray diffraction experiments proved that the occurred austenite lattice expansion - due to nitrogen atoms - depended on the crystallographic direction. The cross-sectional transmission electron microscopy studies showed that the layer consisted of a single cubic phase that contained a lot of defects such as dislocations, stacking faults, slip bands and twins. The high-resolution electron microscopy observations were applied to study the defect formation due to the nitriding process. It was shown that the presence of great number of stacking faults leads to formation of nanotwins. Weak, forbidden {100} reflections were still another characteristic feature of the S-phase. These were not detected in the X-ray spectra of the phase. Basing on the high-resolution electron microscopy studies it can be suggested that the short-range ordering of the nitrogen atoms in the octahedral sites inside the f.c.c. matrix lattice takes place and gives rise to appearance of these spots. It is suggested that the cubic lattice undergoes not only expansion but also slight rombohedral distortion that explains differences in the lattice expansion for different crystallographic directions.

Interface Engineering of Monolayer MoS2/GaN Hybrid Heterostructure: Modified Band Alignment for Photocatalytic Water Splitting Application by Nitridation Treatment.

PubMed

Zhang, Zhaofu; Qian, Qingkai; Li, Baikui; Chen, Kevin J

2018-05-23

Interface engineering is a key strategy to deal with the two-dimensional (2D)/three-dimensional (3D) hybrid heterostructure, since the properties of this atomic-layer-thick 2D material can easily be impacted by the substrate environment. In this work, the structural, electronic, and optical properties of the 2D/3D heterostructure of monolayer MoS 2 on wurtzite GaN surface without and with nitridation interfacial layer are systematically investigated by first-principles calculation and experimental analysis. The nitridation interfacial layer can be introduced into the 2D/3D heterostructure by remote N 2 plasma treatment to GaN sample surface prior to stacking monolayer MoS 2 on top. The calculation results reveal that the 2D/3D integrated heterostructure is energetically favorable with a negative formation energy. Both interfaces demonstrate indirect band gap, which is a benefit for longer lifetime of the photoexcited carriers. Meanwhile, the conduction band edge and valence band edge of the MoS 2 side increases after nitridation treatment. The modification to band alignment is then verified by X-ray photoelectron spectroscopy measurement on MoS 2 /GaN heterostructures constructed by a modified wet-transfer technique, which indicates that the MoS 2 /GaN heterostructure without nitridation shows a type-II alignment with a conduction band offset (CBO) of only 0.07 eV. However, by the deployment of interface nitridation, the band edges of MoS 2 move upward for ∼0.5 eV as a result of the nitridized substrate property. The significantly increased CBO could lead to better electron accumulation capability at the GaN side. The nitridized 2D/3D heterostructure with effective interface treatment exhibits a clean band gap and substantial optical absorption ability and could be potentially used as practical photocatalyst for hydrogen generation by water splitting using solar energy.

Using Noise and Fluctuations for In Situ Measurements of Nitrogen Diffusion Depth.

PubMed

Samoila, Cornel; Ursutiu, Doru; Schleer, Walter-Harald; Jinga, Vlad; Nascov, Victor

2016-10-05

In manufacturing processes involving diffusion (of C, N, S, etc.), the evolution of the layer depth is of the utmost importance: the success of the entire process depends on this parameter. Currently, nitriding is typically either calibrated using a "post process" method or controlled via indirect measurements (H2, O2, H2O + CO2). In the absence of "in situ" monitoring, any variation in the process parameters (gas concentration, temperature, steel composition, distance between sensors and furnace chamber) can cause expensive process inefficiency or failure. Indirect measurements can prevent process failure, but uncertainties and complications may arise in the relationship between the measured parameters and the actual diffusion process. In this paper, a method based on noise and fluctuation measurements is proposed that offers direct control of the layer depth evolution because the parameters of interest are measured in direct contact with the nitrided steel (represented by the active electrode). The paper addresses two related sets of experiments. The first set of experiments consisted of laboratory tests on nitrided samples using Barkhausen noise and yieded a linear relationship between the frequency exponent in the Hooge equation and the nitriding time. For the second set, a specific sensor based on conductivity noise (at the nitriding temperature) was built for shop-floor experiments. Although two different types of noise were measured in these two sets of experiments, the use of the frequency exponent to monitor the process evolution remained valid.

Interface formation in monolayer graphene-boron nitride heterostructures.

PubMed

Sutter, P; Cortes, R; Lahiri, J; Sutter, E

2012-09-12

The ability to control the formation of interfaces between different materials has become one of the foundations of modern materials science. With the advent of two-dimensional (2D) crystals, low-dimensional equivalents of conventional interfaces can be envisioned: line boundaries separating different materials integrated in a single 2D sheet. Graphene and hexagonal boron nitride offer an attractive system from which to build such 2D heterostructures. They are isostructural, nearly lattice-matched, and isoelectronic, yet their different band structures promise interesting functional properties arising from their integration. Here, we use a combination of in situ microscopy techniques to study the growth and interface formation of monolayer graphene-boron nitride heterostructures on ruthenium. In a sequential chemical vapor deposition process, boron nitride grows preferentially at the edges of existing monolayer graphene domains, which can be exploited for synthesizing continuous 2D membranes of graphene embedded in boron nitride. High-temperature growth leads to intermixing near the interface, similar to interfacial alloying in conventional heterostructures. Using real-time microscopy, we identify processes that eliminate this intermixing and thus pave the way to graphene-boron nitride heterostructures with atomically sharp interfaces.

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

NASA Technical Reports Server (NTRS)

Gill, A.

1983-01-01

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.

Molten tin reprocessing of spent nuclear fuel elements

DOEpatents

Heckman, Richard A.

1983-01-01

A method and apparatus for reprocessing spent nuclear fuel is described. Within a containment vessel, a solid plug of tin and nitride precipitates supports a circulating bath of liquid tin therein. Spent nuclear fuel is immersed in the liquid tin under an atmosphere of nitrogen, resulting in the formation of nitride precipitates. The layer of liquid tin and nitride precipitates which interfaces the plug is solidified and integrated with the plug. Part of the plug is melted, removing nitride precipitates from the containment vessel, while a portion of the plug remains solidified to support the liquid tin and nitride precipitates remaining in the containment vessel. The process is practiced numerous times until substantially all of the precipitated nitrides are removed from the containment vessel.

COATED CARBON ELEMENT FOR USE IN NUCLEAR REACTORS AND THE PROCESS OF MAKING THE ELEMENT

DOEpatents

Pyle, R.J.; Allen, G.L.

1963-01-15

S>This patent relates to a carbide-nitride-carbide coating for carbon bodies that are to be subjected to a high temperature nuclear reactor atmosphere, and a method of applying the same. This coating is a highly efficient diffusion barrier and protects the C body from corrosion and erosion by the reactor atmosphere. Preferably, the innermost coating is Zr carbide, the middle coatlng is Zr nitride, and the outermost coating is a mixture of Zr and Nb carbide. The nitride coating acts as a diffusion barrier, while the innermost carbide bonds the nitride to the C body and prevents deleterious reaction between the nitride and C body. The outermost carbide coating protects the nitride coating from the reactor atmosphere. (AEC)

Continuous Fiber Ceramic Composite (CFCC) Program: Gaseous Nitridation

DOE Office of Scientific and Technical Information (OSTI.GOV)

R. Suplinskas G. DiBona; W. Grant

2001-10-29

Textron has developed a mature process for the fabrication of continuous fiber ceramic composite (CFCC) tubes for application in the aluminum processing and casting industry. The major milestones in this project are System Composition; Matrix Formulation; Preform Fabrication; Nitridation; Material Characterization; Component Evaluation

Growth features and spectroscopic structure investigations of nanoprofiled AlN films formed on misoriented GaAs substrates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Seredin, P. V., E-mail: paul@phys.vsu.ru; Goloshchapov, D. L.; Lenshin, A. S.

Nanostructured aluminum-nitride films are formed by reactive ion-plasma sputtering onto GaAs substrates with different orientations. The properties of the films are studied via structural analysis, atomic force microscopy, and infrared and visible–ultraviolet spectroscopy. The aluminum-nitride films can have a refractive index in the range of 1.6–4.0 at a wavelength of ~250 nm and an optical band gap of ~5 eV. It is shown that the morphology, surface composition, and optical characteristics of AlN/GaAs heterophase systems can be controlled using misoriented GaAs substrates.

Protective coatings for high-temperature polymer matrix composites

NASA Technical Reports Server (NTRS)

Harding, David R.; Sutter, James K.; Papadopoulos, Demetrios S.

1993-01-01

Plasma-enhanced chemical vapor deposition was used to deposit silicon nitride on graphite-fiber-reinforced polyimide composites to protect against oxidation at elevated temperatures. The adhesion and integrity of the coating were evaluated by isothermal aging (371 C for 500 hr) and thermal cycling. The amorphous silicon nitride (a-SiN:H) coating could withstand stresses ranging from approximately 0.18 GPa (tensile) to -1.6 GPa (compressive) and provided a 30 to 80 percent reduction in oxidation-induced weight loss. The major factor influencing the effectiveness of a-SiN:H as a barrier coating against oxidation is the surface finish of the polymer composite.

Effects of the Treating Time on Microstructure and Erosion Corrosion Behavior of Salt-Bath-Nitrided 17-4PH Stainless Steel

NASA Astrophysics Data System (ADS)

Wang, Jun; Lin, Yuanhua; Li, Mingxing; Fan, Hongyuan; Zeng, Dezhi; Xiong, Ji

2013-08-01

The effects of salt-bath nitriding time on the microstructure, microhardness, and erosion-corrosion behavior of nitrided 17-4PH stainless steel at 703 K (430 °C) were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and erosion-corrosion testing. The experimental results revealed that the microstructure and phase constituents of the nitrided surface alloy are highly process condition dependent. When 17-4PH stainless steel was subjected to complex salt-bathing nitriding, the main phase of the nitrided layer was expanded martensite ( α`), expanded austenite (S), CrN, Fe4N, and Fe2N. The thickness of nitrided layers increased with the treating time. The salt-bath nitriding improves effectively the surface hardness. The maximum values measured from the treated surface are observed to be 1100 HV0.1 for 40 hours approximately, which is about 3.5 times as hard as the untreated material (309 HV0.1). Low-temperature nitriding can improve the erosion-corrosion resistance against two-phase flow. The sample nitrided for 4 hours has the best corrosion resistance.

Rational design of metal nitride redox materials for solar-driven ammonia synthesis.

PubMed

Michalsky, Ronald; Pfromm, Peter H; Steinfeld, Aldo

2015-06-06

Fixed nitrogen is an essential chemical building block for plant and animal protein, which makes ammonia (NH3) a central component of synthetic fertilizer for the global production of food and biofuels. A global project on artificial photosynthesis may foster the development of production technologies for renewable NH3 fertilizer, hydrogen carrier and combustion fuel. This article presents an alternative path for the production of NH3 from nitrogen, water and solar energy. The process is based on a thermochemical redox cycle driven by concentrated solar process heat at 700-1200°C that yields NH3 via the oxidation of a metal nitride with water. The metal nitride is recycled via solar-driven reduction of the oxidized redox material with nitrogen at atmospheric pressure. We employ electronic structure theory for the rational high-throughput design of novel metal nitride redox materials and to show how transition-metal doping controls the formation and consumption of nitrogen vacancies in metal nitrides. We confirm experimentally that iron doping of manganese nitride increases the concentration of nitrogen vacancies compared with no doping. The experiments are rationalized through the average energy of the dopant d-states, a descriptor for the theory-based design of advanced metal nitride redox materials to produce sustainable solar thermochemical ammonia.

Rational design of metal nitride redox materials for solar-driven ammonia synthesis

PubMed Central

Michalsky, Ronald; Pfromm, Peter H.; Steinfeld, Aldo

2015-01-01

Fixed nitrogen is an essential chemical building block for plant and animal protein, which makes ammonia (NH3) a central component of synthetic fertilizer for the global production of food and biofuels. A global project on artificial photosynthesis may foster the development of production technologies for renewable NH3 fertilizer, hydrogen carrier and combustion fuel. This article presents an alternative path for the production of NH3 from nitrogen, water and solar energy. The process is based on a thermochemical redox cycle driven by concentrated solar process heat at 700–1200°C that yields NH3 via the oxidation of a metal nitride with water. The metal nitride is recycled via solar-driven reduction of the oxidized redox material with nitrogen at atmospheric pressure. We employ electronic structure theory for the rational high-throughput design of novel metal nitride redox materials and to show how transition-metal doping controls the formation and consumption of nitrogen vacancies in metal nitrides. We confirm experimentally that iron doping of manganese nitride increases the concentration of nitrogen vacancies compared with no doping. The experiments are rationalized through the average energy of the dopant d-states, a descriptor for the theory-based design of advanced metal nitride redox materials to produce sustainable solar thermochemical ammonia. PMID:26052421

Growth of single-layer boron nitride dome-shaped nanostructures catalysed by iron clusters.

PubMed

Torre, A La; Åhlgren, E H; Fay, M W; Ben Romdhane, F; Skowron, S T; Parmenter, C; Davies, A J; Jouhannaud, J; Pourroy, G; Khlobystov, A N; Brown, P D; Besley, E; Banhart, F

2016-08-11

We report on the growth and formation of single-layer boron nitride dome-shaped nanostructures mediated by small iron clusters located on flakes of hexagonal boron nitride. The nanostructures were synthesized in situ at high temperature inside a transmission electron microscope while the e-beam was blanked. The formation process, typically originating at defective step-edges on the boron nitride support, was investigated using a combination of transmission electron microscopy, electron energy loss spectroscopy and computational modelling. Computational modelling showed that the domes exhibit a nanotube-like structure with flat circular caps and that their stability was comparable to that of a single boron nitride layer.

Thermal insulation for high temperature microwave sintering operations and method thereof

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Morrow, Marvin S.

1995-01-01

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering.

Method of preparing thermal insulation for high temperature microwave sintering operations

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Morrow, Marvin S.

1996-01-01

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering.

Low-temperature nitridation of manganese and iron oxides using NaNH2 molten salt.

PubMed

Miura, Akira; Takei, Takahiro; Kumada, Nobuhiro

2013-10-21

Manganese and iron nitrides are important functional materials, but their synthesis processes from oxides often require high temperatures. Herein, we show a novel meta-synthesis method for manganese and iron nitrides by low-temperature nitridation of their oxides using NaNH2 molten salt as the nitrogen source in an autoclave at 240 °C. With this method, nitridation of micrometer-sized oxide particles kept their initial morphologies, but the size of the primary particles decreased. The thermodynamic driving force is considered to be the conversion of oxides to sodium hydroxide, and the kinetic of nitridation is improved by the decrease of particle size and the low melting point of NaNH2. This technique as developed here has the advantages of low reaction temperature, reduced consumption of ammonia, employing nonspecialized equipment, and providing facile control of the reactions for producing nitrides from oxides.

Using Noise and Fluctuations for In Situ Measurements of Nitrogen Diffusion Depth

PubMed Central

Samoila, Cornel; Ursutiu, Doru; Schleer, Walter-Harald; Jinga, Vlad; Nascov, Victor

2016-01-01

In manufacturing processes involving diffusion (of C, N, S, etc.), the evolution of the layer depth is of the utmost importance: the success of the entire process depends on this parameter. Currently, nitriding is typically either calibrated using a “post process” method or controlled via indirect measurements (H2, O2, H2O + CO2). In the absence of “in situ” monitoring, any variation in the process parameters (gas concentration, temperature, steel composition, distance between sensors and furnace chamber) can cause expensive process inefficiency or failure. Indirect measurements can prevent process failure, but uncertainties and complications may arise in the relationship between the measured parameters and the actual diffusion process. In this paper, a method based on noise and fluctuation measurements is proposed that offers direct control of the layer depth evolution because the parameters of interest are measured in direct contact with the nitrided steel (represented by the active electrode). The paper addresses two related sets of experiments. The first set of experiments consisted of laboratory tests on nitrided samples using Barkhausen noise and yielded a linear relationship between the frequency exponent in the Hooge equation and the nitriding time. For the second set, a specific sensor based on conductivity noise (at the nitriding temperature) was built for shop-floor experiments. Although two different types of noise were measured in these two sets of experiments, the use of the frequency exponent to monitor the process evolution remained valid. PMID:28773941

Plasma-assisted interface engineering of boron nitride nanostructure films.

PubMed

Pakdel, Amir; Bando, Yoshio; Golberg, Dmitri

2014-10-28

Today many aspects of science and technology are progressing into the nanoscale realm where surfaces and interfaces are intrinsically important in determining properties and performances of materials and devices. One familiar phenomenon in which interfacial interactions play a major role is the wetting of solids. In this work we use a facile one-step plasma method to control the wettability of boron nitride (BN) nanostructure films via covalent chemical functionalization, while their surface morphology remains intact. By tailoring the concentration of grafted hydroxyl groups, superhydrophilic, hydrophilic, and hydrophobic patterns are created on the initially superhydrophobic BN nanosheet and nanotube films. Moreover, by introducing a gradient of the functional groups, directional liquid spreading toward increasing [OH] content is achieved on the films. The resulting insights are meant to illustrate great potentials of this method to tailor wettability of ceramic films, control liquid flow patterns for engineering applications such as microfluidics and biosensing, and improve the interfacial contact and adhesion in nanocomposite materials.

Fabrication and Physical Properties of Titanium Nitride/Hydroxyapatite Composites on Polyether Ether Ketone by RF Magnetron Sputtering Technique

NASA Astrophysics Data System (ADS)

Nupangtha, W.; Boonyawan, D.

2017-09-01

Titanium nitride (TiN) coatings have been used very successfully in a variety of applications because of their excellent properties, such as the high hardness meaning good wear resistance and also used for covering medical implants. Hydroxyapatite is a bioactive ceramic that contributes to the restoration of bone tissue, which together with titanium nitride may contribute to obtaining a superior composite in terms of mechanical and bone tissue interaction matters. This paper aims to explain how to optimize deposition conditions for films synthesis on PEEK by varying sputtering parameters such as nitrogen flow rate and direction, deposition time, d-s (target-to-substrate distance) and 13.56 MHz RF power. The plasma conditions used to deposit films were monitored by the optical emission spectroscopy (OES). Titanium nitride/Hydroxyapatite composite films were performed by gas mixture with nitrogen and argon ratio of 1:3 and target-to-substrate distance at 8 cm. The gold colour, as-deposited film was found on PEEK with high hardness and higher surface energy than uncoated PEEK. X-ray diffraction characterization study was carried to study the crystal structural properties of these composites.

Tribological properties of boron nitride synthesized by ion beam deposition

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.; Spalvins, T.

1985-01-01

The adhesion and friction behavior of boron nitride films on 440 C bearing stainless steel substrates was examined. The thin films containing the boron nitride were synthesized using an ion beam extracted from a borazine plasma. Sliding friction experiments were conducted with BN in sliding contact with itself and various transition metals. It is indicated that the surfaces of atomically cleaned BN coating film contain a small amount of oxides and carbides, in addition to boron nitride. The coefficients of friction for the BN in contact with metals are related to the relative chemical activity of the metals. The more active the metal, the higher is the coefficient of friction. The adsorption of oxygen on clean metal and BN increases the shear strength of the metal - BN contact and increases the friction. The friction for BN-BN contact is a function of the shear strength of the elastic contacts. Clean BN surfaces exhibit relatively strong interfacial adhesion and high friction. The presence of adsorbates such as adventitious carbon contaminants on the BN surfaces reduces the shear strength of the contact area. In contrast, chemically adsorbed oxygen enhances the shear strength of the BN-BN contact and increases the friction.

Process for synthesizing titanium carbide, titanium nitride and titanium carbonitride

DOEpatents

Koc, Rasit; Glatzmaier, Gregory C.

1995-01-01

A process for synthesizing titanium carbide, titanium nitride or titanium carbonitride. The process comprises placing particles of titanium, a titanium salt or titanium dioxide within a vessel and providing a carbon-containing atmosphere within the vessel. The vessel is heated to a pyrolysis temperature sufficient to pyrolyze the carbon to thereby coat the particles with a carbon coating. Thereafter, the carbon-coated particles are heated in an inert atmosphere to produce titanium carbide, or in a nitrogen atmosphere to produce titanium nitride or titanium carbonitride, with the heating being of a temperature and time sufficient to produce a substantially complete solid solution.

Process for synthesizing titanium carbide, titanium nitride and titanium carbonitride

DOEpatents

Koc, R.; Glatzmaier, G.C.

1995-05-23

A process is disclosed for synthesizing titanium carbide, titanium nitride or titanium carbonitride. The process comprises placing particles of titanium, a titanium salt or titanium dioxide within a vessel and providing a carbon-containing atmosphere within the vessel. The vessel is heated to a pyrolysis temperature sufficient to pyrolyze the carbon to thereby coat the particles with a carbon coating. Thereafter, the carbon-coated particles are heated in an inert atmosphere to produce titanium carbide, or in a nitrogen atmosphere to produce titanium nitride or titanium carbonitride, with the heating being of a temperature and time sufficient to produce a substantially complete solid solution.

Process for producing wurtzitic or cubic boron nitride

DOEpatents

Holt, J.B.; Kingman, D.D.; Bianchini, G.M.

1992-04-28

Disclosed is a process for producing wurtzitic or cubic boron nitride comprising the steps of: [A] preparing an intimate mixture of powdered boron oxide, a powdered metal selected from the group consisting of magnesium or aluminum, and a powdered metal azide; [B] igniting the mixture and bringing it to a temperature at which self-sustaining combustion occurs; [C] shocking the mixture at the end of the combustion thereof with a high pressure wave, thereby forming as a reaction product, wurtzitic or cubic boron nitride and occluded metal oxide; and, optionally [D] removing the occluded metal oxide from the reaction product. Also disclosed are reaction products made by the process described.

Process for producing wurtzitic or cubic boron nitride

DOEpatents

Holt, J. Birch; Kingman, deceased, Donald D.; Bianchini, Gregory M.

1992-01-01

Disclosed is a process for producing wurtzitic or cubic boron nitride comprising the steps of: [A] preparing an intimate mixture of powdered boron oxide, a powdered metal selected from the group consisting of magnesium or aluminum, and a powdered metal azide; [B] igniting the mixture and bringing it to a temperature at which self-sustaining combustion occurs; [C] shocking the mixture at the end of the combustion thereof with a high pressure wave, thereby forming as a reaction product, wurtzitic or cubic boron nitride and occluded metal oxide; and, optionally [D] removing the occluded metal oxide from the reaction product. Also disclosed are reaction products made by the process described.

High mobility and high stability glassy metal-oxynitride materials and devices

NASA Astrophysics Data System (ADS)

Lee, Eunha; Kim, Taeho; Benayad, Anass; Hur, Jihyun; Park, Gyeong-Su; Jeon, Sanghun

2016-04-01

In thin film technology, future semiconductor and display products with high performance, high density, large area, and ultra high definition with three-dimensional functionalities require high performance thin film transistors (TFTs) with high stability. Zinc oxynitride, a composite of zinc oxide and zinc nitride, has been conceded as a strong substitute to conventional semiconductor film such as silicon and indium gallium zinc oxide due to high mobility value. However, zinc oxynitride has been suffered from poor reproducibility due to relatively low binding energy of nitrogen with zinc, resulting in the instability of composition and its device performance. Here we performed post argon plasma process on zinc oxynitride film, forming nano-crystalline structure in stable amorphous matrix which hampers the reaction of oxygen with zinc. Therefore, material properties and device performance of zinc oxynitride are greatly enhanced, exhibiting robust compositional stability even exposure to air, uniform phase, high electron mobility, negligible fast transient charging and low noise characteristics. Furthermore, We expect high mobility and high stability zinc oxynitride customized by plasma process to be applicable to a broad range of semiconductor and display devices.

Preparation of refractory cermet structures for lithium compatibility testing

NASA Technical Reports Server (NTRS)

Heestand, R. L.; Jones, R. A.; Wright, T. R.; Kizer, D. E.

1973-01-01

High-purity nitride and carbide cermets were synthesized for compatability testing in liquid lithium. A process was developed for the preparation of high-purity hafnium nitride powder, which was subsequently blended with tungsten powder or tantalum nitride and tungsten powders and fabricated into 3 in diameter billets by uniaxial hot pressing. Specimens were then cut from the billets for compatability testing. Similar processing techniques were applied to produce hafnium carbide and zirconium carbide cermets for use in the testing program. All billets produced were characterized with respect to chemistry, structure, density, and strength properties.

Efficient boron nitride nanotube formation via combined laser-gas flow levitation

DOEpatents

Whitney, R. Roy; Jordan, Kevin; Smith, Michael

2014-03-18

A process for producing boron nitride nanotubes and/or boron-carbon-nitrogen nanotubes of the general formula B.sub.xC.sub.yN.sub.z. The process utilizes a combination of laser light and nitrogen gas flow to support a boron ball target during heating of the boron ball target and production of a boron vapor plume which reacts with nitrogen or nitrogen and carbon to produce boron nitride nanotubes and/or boron-carbon-nitrogen nanotubes of the general formula B.sub.xC.sub.yN.sub.z.

Efficient Boron Nitride Nanotube Formation via Combined Laser-Gas Flow Levitation

NASA Technical Reports Server (NTRS)

Whitney, R. Roy (Inventor); Jordan, Kevin (Inventor); Smith, Michael W. (Inventor)

2014-01-01

A process for producing boron nitride nanotubes and/or boron-carbon-nitrogen nanotubes of the general formula B(sub x)C(sub y)N(sub z) The process utilizes a combination of laser light and nitrogen gas flow to support a boron ball target during heating of the boron ball target and production of a boron vapor plume which reacts with nitrogen or nitrogen and carbon to produce boron nitride nanotubes and/or boron-carbon-nitrogen nanotubes of the general formula B(sub x)C(sub y)N(sub z).

Experimental studies of radiation resistance of boron nitride, C2C ceramics Al2O3 and carbon-fiber composites using a PF-1000 plasma-focus device

NASA Astrophysics Data System (ADS)

Gribkov, V. A.; Tuniz, C.; Demina, E. V.; Dubrovsky, A. V.; Pimenov, V. N.; Maslyaev, S. V.; Gaffka, R.; Gryaznevich, M.; Skladnik-Sadowska, E.; Sadowski, M. J.; Miklaszewski, R.; Paduch, M.; Scholz, M.

2011-04-01

This paper reports on experiments undertaken to compare the radiation resistance of two types of ceramics, boron nitride (BN) and pure alumina (Al2O3), which are used in a TAEA antenna coil installed in the MAST spherical tokamak. Samples of the investigated materials (bulk BN and a 20 μm film of Al2O3 on Al substrate) were exposed on the axis of the plasma-focus PF-1000 device, which can emit intense streams of hot plasma (v≈107 cm s-1 and Npl≈1018 cm-3) and fast deuteron beams (Ei≈100 keV). The most powerful plasma-ion pulse lasted 0.2-1.0 μs and its intensity decayed in about 100 μs. The irradiation process was diagnosed using fast optical cameras, laser interferometry and optical spectrometry. Experiments were performed at power flux densities equal to 109-1010 W cm-2 or 108-109 W cm-2 during the most powerful stage of the interaction process. The irradiated specimens were investigated by means of optical microscopy and x-ray structure analysis (XRSA). It was shown that at 1010 W cm-2 pulses the Al2O3 coating was completely evaporated, whereas a surface of the BN sample became smoother than in the virgin one. A direct comparison of both samples after the action of 108 W cm-2 pulses demonstrated a wave-like structure (more distinct on Al2O3). Weighing of these samples showed, however, that the evaporation of BN was about two times stronger than that of Al2O3 in spite of the lower irradiation flux; the XRSA showed no evidence of cracking of Al2O3 after these pulses. The insulation properties of Al2O3 did not decline, and the Al2O3 coating may be potentially more beneficial, provided that it is kept below its melting point. Characteristic features of damages of a material based on the carbon-fiber composite with additions of silicium carbide (SiC; 8-40% volumetric) were also investigated. It was found that at q=109 W cm-2, the surface erosion is associated with sputtering and evaporation. The degree of this erosion depends on the fibers' orientation in relation to the direction of the plasma-ion streams, and on the percentage of the SiC admixture.

Methods for and products of processing nanostructure nitride, carbonitride and oxycarbonitride electrode power materials by utilizing sol gel technology for supercapacitor applications

DOEpatents

Huang, Yuhong; Wei, Oiang; Chu, Chung-tse; Zheng, Haixing

2001-01-01

Metal nitride, carbonitride, and oxycarbonitride powder with high surface area (up to 150 m.sup.2 /g) is prepared by using sol-gel process. The metal organic precursor, alkoxides or amides, is synthesized firstly. The metal organic precursor is modified by using unhydrolyzable organic ligands or templates. A wet gel is formed then by hydrolysis and condensation process. The solvent in the wet gel is then be removed supercritically to form porous amorphous hydroxide. This porous hydroxide materials is sintered to 725.degree. C. under the ammonia flow and porous nitride powder is formed. The other way to obtain high surface area nitride, carbonitride, and oxycarbonitride powder is to pyrolyze polymerized templated metal amides aerogel in an inert atmosphere. The electrochemical capacitors are prepared by using sol-gel prepared nitride, carbonitride, and oxycarbonitride powder. Two methods are used to assemble the capacitors. Electrode is formed either by pressing the mixture of nitride powder and binder to a foil, or by depositing electrode coating onto metal current collector. The binder or coating is converted into a continuous network of electrode material after thermal treatment to provide enhanced energy and power density. Liquid electrolyte is soaked into porous electrode. The electrochemical capacitor assembly further has a porous separator layer between two electrodes/electrolyte and forming a unit cell.

Mechanical properties of nitrogen-rich surface layers on SS304 treated by plasma immersion ion implantation

NASA Astrophysics Data System (ADS)

Fernandes, B. B.; Mändl, S.; Oliveira, R. M.; Ueda, M.

2014-08-01

The formation of hard and wear resistant surface regions for austenitic stainless steel through different nitriding and nitrogen implantation processes at intermediate temperatures is an established technology. As the inserted nitrogen remains in solid solution, an expanded austenite phase is formed, accounting for these surface improvements. However, experiments on long-term behavior and exact wear processes within the expanded austenite layer are still missing. Here, the modified layers were produced using plasma immersion ion implantation with nitrogen gas and had a thickness of up to 4 μm, depending on the processing temperature. Thicker layers or those with higher surface nitrogen contents presented better wear resistance, according to detailed microscopic investigation on abrasion, plastic deformation, cracking and redeposition of material inside the wear tracks. At the same time, cyclic fatigue testing employing a nanoindenter equipped with a diamond ball was carried out at different absolute loads and relative unloadings. As the stress distribution between the modified layer and the substrate changes with increasing load, additional simulations were performed for obtaining these complex stress distributions. While high nitrogen concentration and/or thicker layers improve the wear resistance and hardness, these modifications simultaneously reduce the surface fatigue resistance.

Methods for improved growth of group III nitride buffer layers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Melnik, Yurity; Chen, Lu; Kojiri, Hidehiro

Methods are disclosed for growing high crystal quality group III-nitride epitaxial layers with advanced multiple buffer layer techniques. In an embodiment, a method includes forming group III-nitride buffer layers that contain aluminum on suitable substrate in a processing chamber of a hydride vapor phase epitaxy processing system. A hydrogen halide or halogen gas is flowing into the growth zone during deposition of buffer layers to suppress homogeneous particle formation. Some combinations of low temperature buffers that contain aluminum (e.g., AlN, AlGaN) and high temperature buffers that contain aluminum (e.g., AlN, AlGaN) may be used to improve crystal quality and morphologymore » of subsequently grown group III-nitride epitaxial layers. The buffer may be deposited on the substrate, or on the surface of another buffer. The additional buffer layers may be added as interlayers in group III-nitride layers (e.g., GaN, AlGaN, AlN).« less

Process for producing ceramic nitrides and carbonitrides and their precursors

DOEpatents

Brown, Gilbert M.; Maya, Leon

1988-01-01

A process for preparing ceramic nitrides and carbonitrides in the form of very pure, fine particulate powder. Appropriate precursor is prepared by reacting a transition metal alkylamide with ammonia to produce a mixture of metal amide and metal imide in the form of an easily pyrolyzable precipitate.

Tunable hole injection of solution-processed polymeric carbon nitride towards efficient organic light-emitting diode

NASA Astrophysics Data System (ADS)

Zhang, Xiaowen; Zheng, Qinghong; Tang, Zhenyu; Li, Wanshu; Zhang, Yan; Xu, Kai; Xue, Xiaogang; Xu, Jiwen; Wang, Hua; Wei, Bin

2018-02-01

Polymeric carbon nitride (CNxHy) has been facilely synthesized from dicyandiamide and functions as a solution-processed hole injection layer in organic light-emitting diodes (OLEDs). The measurements using X-ray diffraction, atomic force microscopy, X-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, and impedance spectroscopy elucidate that CNxHy exhibits superior film morphology and extra electric properties such as tailored work function and tunable hole injection. The luminous efficiency of CNxHy-based OLED is found to improve by 76.6% in comparison to the counterpart using favorite solution-processed poly(ethylene dioxythiophene):poly(styrene sulfonate) as the hole injection layer. Our results also pave a way for broadening carbon nitride applications in organic electronics using the solution process.

Method for producing refractory nitrides

DOEpatents

Quinby, Thomas C.

1989-01-24

A process for making fine, uniform metal nitride powders that can be hot pressed or sintered. A metal salt is placed in a solvent with Melamine and warmed until a metal-Melamine compound forms. The solution is cooled and the metal-Melamine precipitate is calcined at a temperature below 700.degree. C. to form the metal nitrides and to avoid formation of the metal oxide.

Molybdenum enhanced low-temperature deposition of crystalline silicon nitride

DOEpatents

Lowden, Richard A.

1994-01-01

A process for chemical vapor deposition of crystalline silicon nitride which comprises the steps of: introducing a mixture of a silicon source, a molybdenum source, a nitrogen source, and a hydrogen source into a vessel containing a suitable substrate; and thermally decomposing the mixture to deposit onto the substrate a coating comprising crystalline silicon nitride containing a dispersion of molybdenum silicide.

Spin-on metal oxide materials with high etch selectivity and wet strippability

NASA Astrophysics Data System (ADS)

Yao, Huirong; Mullen, Salem; Wolfer, Elizabeth; McKenzie, Douglas; Rahman, Dalil; Cho, JoonYeon; Padmanaban, Munirathna; Petermann, Claire; Hong, SungEun; Her, YoungJun

2016-03-01

Metal oxide or metal nitride films are used as hard mask materials in semiconductor industry for patterning purposes due to their excellent etch resistances against the plasma etches. Chemical vapor deposition (CVD) or atomic layer deposition (ALD) techniques are usually used to deposit the metal containing materials on substrates or underlying films, which uses specialized equipment and can lead to high cost-of-ownership and low throughput. We have reported novel spin-on coatings that provide simple and cost effective method to generate metal oxide films possessing good etch selectivity and can be removed by chemical agents. In this paper, new spin-on Al oxide and Zr oxide hard mask formulations are reported. The new metal oxide formulations provide higher metal content compared to previously reported material of specific metal oxides under similar processing conditions. These metal oxide films demonstrate ultra-high etch selectivity and good pattern transfer capability. The cured films can be removed by various chemical agents such as developer, solvents or wet etchants/strippers commonly used in the fab environment. With high metal MHM material as an underlayer, the pattern transfer process is simplified by reducing the number of layers in the stack and the size of the nano structure is minimized by replacement of a thicker film ACL. Therefore, these novel AZ® spinon metal oxide hard mask materials can potentially be used to replace any CVD or ALD metal, metal oxide, metal nitride or spin-on silicon-containing hard mask films in 193 nm or EUV process.

Atomic-order thermal nitridation of group IV semiconductors for ultra-large-scale integration

NASA Astrophysics Data System (ADS)

Murota, Junichi; Le Thanh, Vinh

2015-03-01

One of the main requirements for ultra-large-scale integration (ULSI) is atomic-order control of process technology. Our concept of atomically controlled processing for group IV semiconductors is based on atomic-order surface reaction control in Si-based CVD epitaxial growth. On the atomic-order surface nitridation of a few nm-thick Ge/about 4 nm-thick Si0.5Ge0.5/Si(100) by NH3, it is found that N atoms diffuse through nm-order thick Ge layer into Si0.5Ge0.5/Si(100) substrate and form Si nitride, even at 500 °C. By subsequent H2 heat treatment, although N atomic amount in Ge layer is reduced drastically, the reduction of the Si nitride is slight. It is suggested that N diffusion in Ge layer is suppressed by the formation of Si nitride and that Ge/atomic-order N layer/Si1-xGex/Si (100) heterostructure is formed. These results demonstrate the capability of CVD technology for atomically controlled nitridation of group IV semiconductors for ultra-large-scale integration. Invited talk at the 7th International Workshop on Advanced Materials Science and Nanotechnology IWAMSN2014, 2-6 November, 2014, Ha Long, Vietnam.

Crystallization of the glassy grain boundary phase in silicon nitride ceramics

NASA Technical Reports Server (NTRS)

Drummond, Charles H., III

1991-01-01

The role was studied of the intergranular glassy phase in silicon nitride as-processed with yttria as a sintering aid. The microstructure, crystallization, and viscosity of the glassy phase were areas studied. Crystallization of the intergranular glassy phase to more refractory crystalline phases should improve the high temperature mechanical properties of the silicon nitride. The addition of a nucleating agent will increase the rate of crystallization. The measurement of the viscosity of the glassy phase will permit the estimation of the high temperature deformation of the silicon nitride.

Endohedral clusterfullerenes--playing with cluster and cage sizes.

PubMed

Dunsch, Lothar; Yang, Shangfeng

2007-06-28

The family of endohedral fullerenes was significantly enlarged within the past six years by the clusterfullerenes containing structures like the M(2)C(2) carbides and the M(3)N nitrides. While the carbide clusters are generated under the standard arc burning conditions according to the stabilisation energy the nitride clusterfullerene type is formed by varying the composition of the cooling gas atmosphere in the arc burning process. The special situation in nitride clusterfullerene synthesis is described in detail and the optimum conditions for the production of nitride clusterfullerenes as the main product in fullerene synthesis are discussed. A review of new nitride clusterfullerenes reported recently is given summarizing the structures, properties and the stability of metal nitride clusterfullerenes. It is shown that all cages with even carbon atoms of C(68) and beyond are available as endohedral nitride clusterstructures. Furthermore the nitride clusterfullerenes are that class of endohedral fullerenes forming the largest number of non-IPR structures. Finally the prospects of this evolving field are briefly discussed taking the superior stability of these endohedral clusterfullerenes into account.

Synthesis of oxide and nitride ceramics in high-power gyrotron discharge

NASA Astrophysics Data System (ADS)

Akhmadullina, N. S.; Skvortsova, N. N.; Obraztsova, E. A.; Stepakhin, V. D.; Konchekov, E. M.; Kargin, Yu F.; Shishilov, O. N.

2017-12-01

Synthesis of oxides, nitrides, and oxynitrides of silicon and aluminium by a pulsed microwave discharge in the mixtures of metal and dielectric powders is described. The microwave pulses were generated by high-power gyrotron (frequency 75 GHz, power up to 550 kW, pulse duration from 0.1 to 15ms). SiO2 + β-Si3N4 (1:1 by molar) and α-Al2O3 + AlN (2:1 by molar) mixtures with Mg (1 and 5wt%) were treated in air with microwave pulses with power of 250÷400 kW and duration of 2÷8 ms. It was found that the discharge cannot be initiated for both mixtures in absence of Mg at any pulse power and duration. When 1% of Mg was added, the discharge was observed for both mixtures under 8 ms pulses of 400 kW; however, the amounts of materials produced were not enough for analysis. With 5% of Mg the discharge was observed for both mixtures under 8 ms pulses of 350 kW, and products of the plasma-chemical processes in the Al2O3 + AlN mixture were analyzed.

Unintentional consequences of dual mode plasma reactors: Implications for upscaling lab-record silicon surface passivation by silicon nitride

NASA Astrophysics Data System (ADS)

Tong, Jingnan; To, Alexander; Lennon, Alison; Hoex, Bram

2017-08-01

Silicon nitride (SiN x ) synthesised by low-temperature plasma enhanced chemical vapour deposition (PECVD) is the most extensively used antireflection coating for crystalline silicon solar cells because of its tunable refractive index in combination with excellent levels of surface and bulk passivation. This has attracted a significant amount of research on developing SiN x films towards an optimal electrical and optical performance. Typically, recipes are first optimised in lab-scale reactors and subsequently, the best settings are transferred to high-throughput reactors. In this paper, we show that for one particular, but widely used, PECVD reactor configuration this upscaling is severely hampered by an important experimental artefact. Specifically, we report on the unintentional deposition of a dual layer structure in a dual mode AK 400 plasma reactor from Roth & Rau which has a significant impact on its surface passivation performance. It is found that the radio frequency (RF) substrate bias ignites an unintentional depositing plasma before the ignition of the main microwave (MW) plasma. This RF plasma deposits a Si-rich intervening SiN x layer (refractive index = 2.4) while using a recipe for stoichiometric SiN x . This layer was found to be 18 nm thick in our case and had an extraordinary impact on the Si surface passivation, witnessed by a reduction in effective surface recombination velocity from 22.5 to 6.2 cm/s. This experimental result may explain some “out of the ordinary” excellent surface passivation results reported recently for nearly stoichiometric SiN x films and has significant consequences when transferring these results to high-throughput deposition systems.

Experience of high-nitrogenous steel powder application in repairs and surface hardening of responsible parts for power equipment by plasma spraying

NASA Astrophysics Data System (ADS)

Kolpakov, A. S.; Kardonina, N. I.

2016-02-01

The questions of the application of novel diffusion-alloying high-nitrogenous steel powders for repair and surface hardening of responsible parts of power equipment by plasma spraying are considered. The appropriateness of the method for operative repair of equipment and increasing its service life is justified. General data on the structure, properties, and manufacture of nitrogen-, aluminum-, and chromium-containing steel powders that are economically alloyed using diffusion are described. It is noted that the nitrogen release during the decomposition of iron nitrides, when heating, protects the powder particles from oxidation in the plasma jet. It is shown that the coating retains 50% of nitrogen that is contained in the powder. Plasma spraying modes for diffusion-alloying high-nitrogenous steel powders are given. The service properties of plasma coatings based on these powders are analyzed. It is shown that the high-nitrogenous steel powders to a nitrogen content of 8.9 wt % provide the necessary wear resistance and hardness of the coating and the strength of its adhesion to the substrate and corrosion resistance to typical aggressive media. It is noted that increasing the coating porosity promotes stress relaxation and increases its thickness being limited with respect to delamination conditions in comparison with dense coatings on retention of the low defectiveness of the interface and high adhesion to the substrate. The examples of the application of high-nitrogenous steel powders in power engineering during equipment repairs by service companies and overhaul subdivisions of heat power plants are given. It is noted that the plasma spraying of diffusion-alloyed high-nitrogenous steel powders is a unique opportunity to restore nitrided steel products.

Growth of 1.5 micron gallium indium nitrogen arsenic antimonide vertical cavity surface emitting lasers by molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Wistey, Mark Allan

Fiber optics has revolutionized long distance communication and long haul networks, allowing unimaginable data speeds and noise-free telephone calls around the world for mere pennies per hour at the trunk level. But the high speeds of optical fiber generally do not extend to individual workstations or to the home, in large part because it has been difficult and expensive to produce lasers which emitted light at wavelengths which could take advantage of optical fiber. One of the most promising solutions to this problem is the development of a new class of semiconductors known as dilute nitrides. Dilute nitrides such as GaInNAs can be grown directly on gallium arsenide, which allows well-established processing techniques. More important, gallium arsenide allows the growth of vertical-cavity surface-emitting lasers (VCSELs), which can be grown in dense, 2D arrays on each wafer, providing tremendous economies of scale for manufacturing, testing, and packaging. Unfortunately, GaInNAs lasers have suffered from what has been dubbed the "nitrogen penalty," with high thresholds and low efficiency as the fraction of nitrogen in the semiconductor was increased. This thesis describes the steps taken to identify and essentially eliminate the nitrogen penalty. Protecting the wafer surface from plasma ignition, using an arsenic cap, greatly improved material quality. Using a Langmuir probe, we further found that the nitrogen plasma source produced a large number of ions which damaged the wafer during growth. The ions were dramatically reduced using deflection plates. Low voltage deflection plates were found to be preferable to high voltages, and simulations showed low voltages to be adequate for ion removal. The long wavelengths from dilute nitrides can be partly explained by wafer damage during growth. As a result of these studies, we demonstrated the first CW, room temperature lasers at wavelengths beyond 1.5mum on gallium arsenide, and the first GaInNAs(Sb) VCSELs beyond 1.31mum: 1.46mum. These techniques offer the promise of inexpensive, high speed fiber networking.

Method of preparing thermal insulation for high temperature microwave sintering operations

DOEpatents

Holcombe, C.E.; Dykes, N.L.; Morrow, M.S.

1996-07-16

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering. 1 fig.

Thermal insulation for high temperature microwave sintering operations and method thereof

DOEpatents

Holcombe, C.E.; Dykes, N.L.; Morrow, M.S.

1995-09-12

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering. 1 fig.

Fabrication of lateral lattice-polarity-inverted GaN heterostructure

NASA Astrophysics Data System (ADS)

Katayama, Ryuji; Kuge, Yoshihiro; Kondo, Takashi; Onabe, Kentaro

2007-04-01

Fabrication of the lateral polarity-inverted GaN heterostructure on sapphire (0 0 0 1) using a radio-frequency plasma enhanced molecular beam epitaxy is demonstrated. Its microscopic properties, which are closely related to the local polarity distribution, such as surface potentials, piezoelectric polarizations and residual carrier concentrations were investigated by Kelvin force microscopy and micro-Raman scattering. The successful inversion from Ga-polarity to N-polarity of GaN in a specific domain and its higher crystal perfection had been confirmed clearly by these microscopic analyses. The results were also fairly consistent with that of KOH etching experiments, which suggest the applicability of these processes to the fabrication of photonic nanostructures composed of nitride semiconductors.

Molybdenum enhanced low-temperature deposition of crystalline silicon nitride

DOEpatents

Lowden, R.A.

1994-04-05

A process for chemical vapor deposition of crystalline silicon nitride is described which comprises the steps of: introducing a mixture of a silicon source, a molybdenum source, a nitrogen source, and a hydrogen source into a vessel containing a suitable substrate; and thermally decomposing the mixture to deposit onto the substrate a coating comprising crystalline silicon nitride containing a dispersion of molybdenum silicide. 5 figures.

Thermal oxidation and nitridation of Si nanowalls prepared by metal assisted chemical etching

NASA Astrophysics Data System (ADS)

Behera, Anil K.; Viswanath, R. N.; Lakshmanan, C.; Polaki, S. R.; Sarguna, R. M.; Mathews, Tom

2018-04-01

Silicon nanowalls with controlled orientation have been prepared using metal assisted chemical etching process. Thermal oxidation and nitridation processes have been carried out on the prepared silicon nanowalls under a control flow of oxygen/nitrogen gases independently at 1050°C for 900s. The morphology and structural properties of the as-prepared, oxidized and nitridated silicon nanowalls have been studied using the scanning electron microscopy and the Grazing incident X-ray diffraction techniques. The results obtained from the analysis of X-ray diffraction patterns and the microscopy images are discussed.

The effect of plasma surface treatment on the bioactivity of titanium implant materials (in vitro)

PubMed Central

Abdelrahim, Ramy A.; Badr, Nadia A.; Baroudi, Kusai

2016-01-01

Background: The surface of an implantable biomaterial plays a very important role in determining the biocompatibility, osteoinduction, and osteointegration of implants because it is in intimate contact with the host bone and soft tissues. Objective: This study was aimed to assess the effect of plasma surface treatment on the bioactivity of titanium alloy (Ti–6Al–4V). Materials and Methods: Fifteen titanium alloy samples were used in this study. The samples were divided into three groups (with five samples in each group). Five samples were kept untreated and served as control (group A). Another five plasma samples were sprayed for nitrogen ion implantation on their surfaces (group B) and the last five samples were pre-etched with acid before plasma treatment (group C). All the investigated samples were immersed for 7 days in Hank's balanced salt solution (HBSS) which was used as a simulating body fluid (SBF) at pH 7.4 and 37°C. HBSS was renewed every 3 days. The different surfaces were characterized by X-ray diffraction (XRD), Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDXA), and Fourier Transformation Infrared Spectroscopy (FTIR). Results: Nitriding of Ti-alloy samples via plasma nitrogen ion implantation increased the bioactivity of titanium. Moreover, the surface topography affected the chemical structure of the formed apatite. Increasing the surface roughness enhanced the bioactivity of the implant material. Conclusions: Nitridation can be exploited as an effective way to promote the formation of bone-like material on the implant surface. PMID:27011927

Method For Processing Spent (Trn,Zr)N Fuel

DOEpatents

Miller, William E.; Richmann, Michael K.

2004-07-27

A new process for recycling spent nuclear fuels, in particular, mixed nitrides of transuranic elements and zirconium. The process consists of two electrorefiner cells in series configuration. A transuranic element such as plutonium is reduced at the cathode in the first cell, zirconium at the cathode in the second cell, and nitrogen-15 is released and captured for reuse to make transuranic and zirconium nitrides.

Plasma enhanced ultrastable self-powered visible-blind deep ultraviolet photodetector based on atomically thin boron nitride sheets

NASA Astrophysics Data System (ADS)

Feng, Peter Xianping; Rivera, Manuel; Velazquez, Rafael; Aldalbahi, Ali

We extend our work on the use of digitally controlled plasma deposition technique to synthesize high quality boron nitride nanosheets (BNNSs). The nanoscale morphologies and layered growth characteristics of the BNNSs were characterized using scanning electron microscope, transmission electron microscopy, and atomic force microscopy. The experimental data indicated each sample consists of multiple atomically thin, highly transparent BNNSs that overlap one another with certain orientations. Purity and structural properties were characterized by Raman scattering, XRD, FTIR and XPS. Based on these characterizations, 2D BNNSs based self-powered, visible blind deep UV detectors were designed, fabricated, and tested. The bias, temperature, and humidity effects on the photocurrent strength were investigated. A significant increase of signal-to-noise ratio after plasma treatment was observed. The fabricated photodetectors presented exceptional properties: a very stable baseline and a high sensitivity to weak intensities of radiation in both UVC and UVB range while remaining visible-blind, a high signal-to-noise ratio, and excellent repeatability even when the operating temperature was up to 400 0C. The shift in cutoff wavelength was also observed. This work is supported by the Army Research Office/DoD Grant (62826-RT-REP) and the ISPP#0058 at King Saud University.

Low threshold field emission from high-quality cubic boron nitride films

NASA Astrophysics Data System (ADS)

Teii, Kungen; Matsumoto, Seiichiro

2012-05-01

Field emission performance of materials with mixed sp2/sp3 phases often depends upon the phase composition at the surface. In this study, the emission performance of high-quality cubic boron nitride (cBN) films is studied in terms of phase purity. Thick cBN films consisting of micron-sized grains are prepared from boron trifluoride gas by chemical vapor deposition in a plasma jet and an inductively coupled plasma. Both the bulk and surface phase purities as well as crystallinities of cBN evaluated by visible and ultraviolet Raman spectroscopy, glancing-angle x-ray diffraction, and x-ray photoelectron spectroscopy are the highest when the film is deposited in a plasma jet under an optimized condition. The emission turn-on field decreases with increasing the phase purity, down to around 5 V/μm for the highest cBN purity, due to the larger field enhancement, while it is higher than 14 V/μm without cBN (sp2-bonded hexagonal BN only). The results indicate that the total field enhancement for the high phase purity film is governed by the internal field amplification related to the surface coverage of more conductive cBN, rather than the external one related to the surface topology or roughness.

Local Dynamics of Chemical Kinetics at Different Phases of Nitriding Process

NASA Astrophysics Data System (ADS)

Özdemir, İ. Bedii; Akar, Firat

2015-08-01

The local dynamics of chemical kinetics at different phases of the nitriding process have been studied. The calculations are performed under the conditions where the temperature and composition data are provided experimentally from an in-service furnace. Results are presented in temporal variations of gas concentrations and the nitrogen coverage on the surface. It is shown that if it is available in the furnace, the adsorption of the N2 gas can seemingly start at temperatures as low as 200 °C. However, at such low temperatures, as the diffusion into the material is very unlikely, this results in the surface poisoning. It becomes clear that, contrary to common knowledge, the nitriding heat treatment with ammonia as a nitrogen-providing medium is possible at temperatures like 400 °C. Under these conditions, however, the presence of excess amounts of product gas N2 in the furnace atmosphere suppresses the forward kinetics in the nitriding process. It seems that the best operating point in the nitriding heat treatment is achieved with a mixture of 6% N2. When the major nitriding species NH3 is substituted by N2 and the N2 fraction increases above 30%, the rate of the forward reaction decreases drastically, so that there is no point to continue the furnace operation any further. Hence, during the initial heating phase, the N2 gas must be purged from the furnace to keep its fraction less than 30% before the furnace reaches the temperature where the reaction starts.

Improved toughness of refractory compounds. [with elimination of the grain boundary phase

NASA Technical Reports Server (NTRS)

Wright, T. R.; Niesz, D. E.

1974-01-01

The concept of grain-boundary-engineering through elimination of the grain-boundary silicate phase in silicon nitride was developed. The process involved removal of the silica from the nitride powder via a thermal treatment coupled with the use of nitride additives to compensate the remaining oxygen. Magnesium and aluminum nitrides are found to be the most effective additive for use as oxygen compensators. Strength decreases at elevated temperatures are not observed in the alumina containing material. The creep rate of a dual additive sialon composition was two orders of magnitude lower at 1400 C than commercial silicon nitride. A cursory analysis of the creep mechanism indicate that grain-boundary sliding is avoided through elimination of the grain-boundary silicate phase.

Study of the kinetics and mechanism of the thermal nitridation of SiO2

NASA Technical Reports Server (NTRS)

Vasquez, R. P.; Madhukar, A.; Grunthaner, F. J.; Naiman, M. L.

1985-01-01

X-ray photoelectron spectroscopy (XPS) has been used to study the nitridation time and temperature dependence of the nitrogen distribution in thermally nitrided SiO2 films. The XPS data show that the maximum nitrogen concentration near the (SiO(x)N(y)/Si interface is initially at the interface, but moves 20-25 A away from the interface with increasing nitridation time. Computer modeling of the kinetic processes involved is carried out and reveals a mechanism in which diffusing species, initially consisting primarily of nitrogen, react with the substrate, followed by formation of the oxygen-rich oxynitride due to reaction of the diffusing oxygen displaced by the slower nitridation of the SiO2. The data are consistent with this mechanism provided the influence of the interfacial strain on the nitridation and oxidation kinetics is explicitly accounted for.

Effect of the hexagonal phase interlayer on rectification properties of boron nitride heterojunctions to silicon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Teii, K., E-mail: teii@asem.kyushu-u.ac.jp; Ito, H.; Katayama, N.

2015-02-07

Rectification properties of boron nitride/silicon p-n heterojunction diodes fabricated under low-energy ion impact by plasma-enhanced chemical vapor deposition are studied in terms of the resistive sp{sup 2}-bonded boron nitride (sp{sup 2}BN) interlayer. A two-step biasing technique is developed to control the fraction of cubic boron nitride (cBN) phase and, hence, the thickness of the sp{sup 2}BN interlayer in the films. The rectification ratio at room temperature is increased up to the order of 10{sup 4} at ±10 V of biasing with increasing the sp{sup 2}BN thickness up to around 130 nm due to suppression of the reverse leakage current. The variation ofmore » the ideality factor in the low bias region is related to the interface disorders and defects, not to the sp{sup 2}BN thickness. The forward current follows the Frenkel-Poole emission model in the sp{sup 2}BN interlayer at relatively high fields when the anomalous effect is assumed. The transport of the minority carriers for reverse current is strongly limited by the high bulk resistance of the thick sp{sup 2}BN interlayer, while that of the major carriers for forward current is much less affected.« less

MBE growth and processing of III/V-nitride semiconductor thin film structures: Growth of gallium indium arsenic nitride and nano-machining with focused ion beam and electron beam

NASA Astrophysics Data System (ADS)

Park, Yeonjoon

The advanced semiconductor material InGaAsN was grown with nitrogen plasma assisted Molecular Beam Epitaxy (MBE). The InGaAsN layers were characterized with High Resolution X-ray Diffraction (HRXDF), Atomic Fore Microscope (AFM), X-ray Photoemission Spectroscopy (XPS) and Photo-Luminescence (PL). The reduction of the band gap energy was observed with the incorporation of nitrogen and the lattice matched condition to the GaAs substrate was achieved with the additional incorporation of indium. A detailed investigation was made for the growth mode changes from planar layer-by-layer growth to 3D faceted growth with a higher concentration of nitrogen. A new X-ray diffraction analysis was developed and applied to the MBE growth on GaAs(111)B, which is one of the facet planes of InGaAsN. As an effort to enhance the processing tools for advanced semiconductor materials, gas assisted Focused Ion Beam (FIB) vertical milling was performed on GaN. The FIB processed area shows an atomically flat surface, which is good enough for the fabrication of Double Bragg Reflector (DBR) mirrors for the Blue GaN Vertical Cavity Surface Emitting Laser (VCSEL) Diodes. An in-situ electron beam system was developed to combine the enhanced lithographic processing capability with the atomic layer growth capability by MBE. The electron beam system has a compensation capability against substrate vibration and thermal drift. In-situ electron beam lithography was performed with the low pressure assisting gas. The advanced processing and characterization methods developed in this thesis will assist the development of superior semiconductor materials for the future.

Raising the Corrosion Resistance of Low-Carbon Steels by Electrolytic-Plasma Saturation with Nitrogen and Carbon

NASA Astrophysics Data System (ADS)

Kusmanov, S. A.; Grishina, E. P.; Belkin, P. N.; Kusmanova, Yu. V.; Kudryakova, N. O.

2017-05-01

Structural features of the external oxide layer and internal nitrided, carbonitrided and carburized layers in steels 10, 20 and St3 produced by the method of electrolytic plasma treatment are studied. Specimens of the steels are tested for corrosion in a naturally aerated 1-N solution of sodium chloride. The condition of the metal/sodium chloride solution interface is studied by the method of electrochemical impedance spectroscopy. It is shown that the corrosion resistance of low-carbon steels can be raised by anode electrolytic-plasma saturation with nitrogen and carbon. Recommendations are given on the choice of carbonitriding modes for structural steels.

Precise control of atomic nitrogen production in an electron cyclotron resonance plasma using N2/noble gas mixtures

NASA Astrophysics Data System (ADS)

Fan, Z. Y.; Newman, N.

1998-07-01

The atomic nitrogen flux and impacting ion kinetic energy are two important parameters which influence the quality of deposited nitride films using reactive growth. In this letter, a method is described to control the flux and kinetic energy of atomic and molecular nitrogen ions using an electron cyclotron resonance plasma with N2/Ar and N2/Ne gas mixtures. The results clearly show that the addition of neon to nitrogen plasma can remarkably enhance the production rate of atomic nitrogen due to Penning ionization involving the metastable state of Ne. In contrast, the addition of argon significantly decreases the rate.

Paramagnetic defects and charge trapping behavior of ZrO2 films deposited on germanium by plasma-enhanced CVD

NASA Astrophysics Data System (ADS)

Mahata, C.; Bera, M. K.; Bose, P. K.; Maiti, C. K.

2009-02-01

Internal photoemission and magnetic resonance studies have been performed to investigate the charge trapping behavior and chemical nature of defects in ultrathin (~14 nm) high-k ZrO2 dielectric films deposited on p-Ge (1 0 0) substrates at low temperature (<200 °C) by plasma-enhanced chemical vapor deposition (PECVD) in a microwave (700 W, 2.45 GHz) plasma at a pressure of ~65 Pa. Both the band and defect-related electron states have been characterized using electron paramagnetic resonance, internal photoemission, capacitance-voltage and current-voltage measurements under UV illumination. Capacitance-voltage and photocurrent-voltage measurements were used to determine the centroid of oxide charge within the high-k gate stack. The observed shifts in photocurrent response of the Al/ZrO2/GeO2/p-Ge metal-insulator-semiconductor (MIS) capacitors indicate the location of the centroids to be within the ZrO2 dielectric near to the gate electrode. Moreover, the measured flat band voltage and photocurrent shifts also indicate a large density of traps in the dielectric. The impact of plasma nitridation on the interfacial quality of the oxides has been investigated. Different N sources, such as NO and NH3, have been used for nitrogen engineering. Oxynitride samples show a lower defect density and trapping over the non-nitrided samples. The charge trapping and detrapping properties of MIS capacitors under stressing in constant current and voltage modes have been investigated in detail.

NbN tunnel junctions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Villegier, J.C.; Goniche, M.; Renard, P.

1985-03-01

All-niobium nitride Josephson junctions have been prepared successfully using a new processing called SNOP: Selective Niobium (Nitride) Overlap Process. Such a process involves the ''trilayer'' deposition on the whole wafer before selective patterning of the electrodes by optically controlled Dry Reactive Ion Etching. Only two photomask levels are need to define an ''overlap'' or a ''cross-type'' junction with a good accuracy. The properties of the niobium nitride films deposited by DC-Magnetron sputtering and the surface oxide growth are analysed. The most critical point to obtain high quality and high gap value junctions resides in the early stage of the NbNmore » counterelectrode growth. Some possibilities to overcome such a handicap exist even if the fabrication needs substrate temperatures below 250/sup 0/C.« less

Ultralow-Threshold Electrically Pumped Quantum-Dot Photonic-Crystal Nanocavity Laser

DTIC Science & Technology

2011-05-01

we demonstrate a quantum-dot photonic-crystal nanocavity laser in gallium arsenide pumped by a lateral p–i–n junction formed by ion implantation...330 nm layer of silicon nitride was then deposited on the sample using plasma-enhanced chemical vapour deposition (PECVD) to serve as a mask for ion

Structural modifications and corrosion behavior of martensitic stainless steel nitrided by plasma immersion ion implantation

NASA Astrophysics Data System (ADS)

Figueroa, C. A.; Alvarez, F.; Zhang, Z.; Collins, G. A.; Short, K. T.

2005-07-01

In this work we report a study of the structural modifications and corrosion behavior of martensitic stainless steels (MSS) nitrided by plasma immersion ion implantation (PI3). The samples were characterized by x-ray diffraction, scanning electron microscopy, energy dispersive x-ray spectroscopy, photoemission electron spectroscopy, and potentiodynamic electrochemical measurements. Depending on the PI3 treatment temperature, three different material property trends are observed. At lower implantation temperatures (e.g., 360 °C), the material corrosion resistance is improved and a compact phase of ɛ-(Fe,Cr)3N, without changes in the crystal morphology, is obtained. At intermediate temperatures (e.g., 430 °C), CrN precipitates form principally at grain boundaries, leading to a degradation in the corrosion resistance compared to the original MSS material. At higher temperatures (e.g., 500 °C), the relatively great mobility of the nitrogen and chromium in the matrix induced random precipitates of CrN, transforming the original martensitic phase into α-Fe (ferrite), and causing a further degradation in the corrosion resistance.

Optical and transport properties of LaTi{sub 1−x}M{sub x}(O,N){sub 3±δ} (x=0; 0.1, M=Nb{sup 5+}, W{sup 6+}) thin films prepared by plasma ammonolysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maegli, Alexandra E.; Sagarna, Leyre; Populoh, Sascha

2014-03-15

Oxynitride thin films of composition LaTi{sub 1−x}M{sub x}(O,N){sub 3±δ} with x=0; 0.1 and M=Nb{sup 5+}, W{sup 6+} were prepared by nitridation via microwave-induced plasma (MIP) ammonolysis, which allowed keeping the nitridation time short (16 min). The higher possible oxidation states of the B-site substituents (Nb{sup 5+}, W{sup 6+}) with respect to Ti{sup 4+} caused higher N content for LaTi{sub 0.9}Nb{sub 0.1}(O,N){sub 3±δ} and LaTi{sub 0.9}W{sub 0.1}(O,N){sub 3±δ} compared to LaTiO{sub 2}N due to charge-compensation. XPS O 1s and N 1s core level and valence band spectra evidenced for increasing N content in the order LaTiO{sub 2}N

Growth of diamond by RF plasma-assisted chemical vapor deposition

NASA Technical Reports Server (NTRS)

Meyer, Duane E.; Ianno, Natale J.; Woollam, John A.; Swartzlander, A. B.; Nelson, A. J.

1988-01-01

A system has been designed and constructed to produce diamond particles by inductively coupled radio-frequency, plasma-assisted chemical vapor deposition. This is a low-pressure, low-temperature process used in an attempt to deposit diamond on substrates of glass, quartz, silicon, nickel, and boron nitride. Several deposition parameters have been varied including substrate temperature, gas concentration, gas pressure, total gas flow rate, RF input power, and deposition time. Analytical methods employed to determine composition and structure of the deposits include scanning electron microscopy, absorption spectroscopy, scanning Auger microprobe spectroscopy, and Raman spectroscopy. Analysis indicates that particles having a thin graphite surface, as well as diamond particles with no surface coatings, have been deposited. Deposits on quartz have exhibited optical bandgaps as high as 4.5 eV. Scanning electron microscopy analysis shows that particles are deposited on a pedestal which Auger spectroscopy indicates to be graphite. This is a phenomenon that has not been previously reported in the literature.

Calibration of high-dynamic-range, finite-resolution x-ray pulse-height spectrometers for extracting electron energy distribution data from the PFRC-2 device

NASA Astrophysics Data System (ADS)

Swanson, C.; Jandovitz, P.; Cohen, S. A.

2017-10-01

Knowledge of the full x-ray energy distribution function (XEDF) emitted from a plasma over a large dynamic range of energies can yield valuable insights about the electron energy distribution function (EEDF) of that plasma and the dynamic processes that create them. X-ray pulse height detectors such as Amptek's X-123 Fast SDD with Silicon Nitride window can detect x-rays in the range of 200eV to 100s of keV. However, extracting EEDF from this measurement requires precise knowledge of the detector's response function. This response function, including the energy scale calibration, the window transmission function, and the resolution function, can be measured directly. We describe measurements of this function from x-rays from a mono-energetic electron beam in a purpose-built gas-target x-ray tube. Large-Z effects such as line radiation, nuclear charge screening, and polarizational Bremsstrahlung are discussed.

Colloidal characterization of silicon nitride and silicon carbide

NASA Technical Reports Server (NTRS)

Feke, Donald L.

1986-01-01

The colloidal behavior of aqueous ceramic slips strongly affects the forming and sintering behavior and the ultimate mechanical strength of the final ceramic product. The colloidal behavior of these materials, which is dominated by electrical interactions between the particles, is complex due to the strong interaction of the solids with the processing fluids. A surface titration methodology, modified to account for this interaction, was developed and used to provide fundamental insights into the interfacial chemistry of these systems. Various powder pretreatment strategies were explored to differentiate between true surface chemistry and artifacts due to exposure history. The colloidal behavior of both silicon nitride and carbide is dominated by silanol groups on the powder surfaces. However, the colloid chemistry of silicon nitride is apparently influenced by an additional amine group. With the proper powder treatments, silicon nitride and carbide powder can be made to appear colloidally equivalent. The impact of these results on processing control will be discussed.

Synthesis of fine-grained .alpha.-silicon nitride by a combustion process

DOEpatents

Holt, J. Birch; Kingman, Donald D.; Bianchini, Gregory M.

1990-01-01

A combustion synthesis process for the preparation of .alpha.-silicon nitride and composites thereof is disclosed. Preparation of the .alpha.-silicon nitride comprises the steps of dry mixing silicon powder with an alkali metal azide, such as sodium azide, cold-pressing the mixture into any desired shape, or loading the mixture into a fused, quartz crucible, loading the crucible into a combustion chamber, pressurizing the chamber with nitrogen and igniting the mixture using an igniter pellet. The method for the preparation of the composites comprises dry mixing silicon powder (Si) or SiO.sub.2, with a metal or metal oxide, adding a small amount of an alkali metal azide such as sodium azide, introducing the mixture into a suitable combustion chamber, pressurizing the combustion chamber with nitrogen, igniting the mixture within the combustion chamber, and isolating the .alpha.-silicon nitride formed as a reaction product.

Effect of Various Heat Treatment Processes on Fatigue Behavior of Tool Steel for Cold Forging Die

NASA Astrophysics Data System (ADS)

Jin, S. U.; Kim, S. S.; Lee, Y. S.; Kwon, Y. N.; Lee, J. H.

Effects of various heat treatment processes, including "Q/T (quenching and tempering)", "Q/CT/T (Quenching, cryogenic treatment and tempering)", "Q/T (quenching and tempering) + Ti-nitriding" and "Q/CT/T (Cryogenic treatment and tempering) + Ti-nitriding", on S-N fatigue behavior of AISI D2 tool steel were investigated. The optical micrographs and Vicker's hardness values at near surface and core area were examined for each specimen. Uniaxial fatigue tests were performed by using an electro-magnetic resonance fatigue testing machine at a frequency of 80 Hz and an R ratio of -1. The overall resistance to fatigue tends to decrease significantly with Ti-nitriding treatment compared to those for the general Q/T and Q/CT/T specimens. The reduced resistance to fatigue with Ti-nitriding is discussed based on the microstructural and fractographic analyses.

Process for producing amorphous and crystalline silicon nitride

DOEpatents

Morgan, P.E.D.; Pugar, E.A.

1985-11-12

A process for producing amorphous or crystalline silicon nitride is disclosed which comprises reacting silicon disulfide ammonia gas at elevated temperature. In a preferred embodiment silicon disulfide in the form of whiskers'' or needles is heated at temperature ranging from about 900 C to about 1,200 C to produce silicon nitride which retains the whisker or needle morphological characteristics of the silicon disulfide. Silicon carbide, e.g. in the form of whiskers, also can be prepared by reacting substituted ammonia, e.g. methylamine, or a hydrocarbon containing active hydrogen-containing groups, such as ethylene, with silicon disulfide, at elevated temperature, e.g. 900 C. 6 figs.

Etching process for improving the strength of a laser-machined silicon-based ceramic article

DOEpatents

Copley, Stephen M.; Tao, Hongyi; Todd-Copley, Judith A.

1991-01-01

A process for improving the strength of laser-machined articles formed of a silicon-based ceramic material such as silicon nitride, in which the laser-machined surface is immersed in an etching solution of hydrofluoric acid and nitric acid for a duration sufficient to remove substantially all of a silicon film residue on the surface but insufficient to allow the solution to unduly attack the grain boundaries of the underlying silicon nitride substrate. This effectively removes the silicon film as a source of cracks that otherwise could propagate downwardly into the silicon nitride substrate and significantly reduce its strength.

Etching process for improving the strength of a laser-machined silicon-based ceramic article

DOEpatents

Copley, S.M.; Tao, H.; Todd-Copley, J.A.

1991-06-11

A process is disclosed for improving the strength of laser-machined articles formed of a silicon-based ceramic material such as silicon nitride, in which the laser-machined surface is immersed in an etching solution of hydrofluoric acid and nitric acid for a duration sufficient to remove substantially all of a silicon film residue on the surface but insufficient to allow the solution to unduly attack the grain boundaries of the underlying silicon nitride substrate. This effectively removes the silicon film as a source of cracks that otherwise could propagate downwardly into the silicon nitride substrate and significantly reduce its strength. 1 figure.

Process for producing amorphous and crystalline silicon nitride

DOEpatents

Morgan, Peter E. D.; Pugar, Eloise A.

1985-01-01

A process for producing amorphous or crystalline silicon nitride is disclosed which comprises reacting silicon disulfide ammonia gas at elevated temperature. In a preferred embodiment silicon disulfide in the form of "whiskers" or needles is heated at temperature ranging from about 900.degree. C. to about 1200.degree. C. to produce silicon nitride which retains the whisker or needle morphological characteristics of the silicon disulfide. Silicon carbide, e.g. in the form of whiskers, also can be prepared by reacting substituted ammonia, e.g. methylamine, or a hydrocarbon containing active hydrogen-containing groups, such as ethylene, with silicon disulfide, at elevated temperature, e.g. 900.degree. C.

Charge retention in scaled SONOS nonvolatile semiconductor memory devices—Modeling and characterization

NASA Astrophysics Data System (ADS)

Hu, Yin; White, Marvin H.

1993-10-01

A new analytical model is developed to investigate the influence of the charge loss processes in the retention mode of the SONOS NVSM device. The model considers charge loss by the following processes: (1) electron back-tunneling from the nitride traps to the Si conduction band, (2) electron back-tunneling from the nitride traps to the Si/SiO 2 interface traps and (3) hole injection from the Si valence band to the nitride traps. An amphoteric trap charge distribution is used in this model. The new charge retention model predicts that process (1) determines the short term retention, while processes (2) and (3) determine the long term retention. Good agreement has been reached between the results of analytical calculations and the experimental retention data on both surface channel and buried channel SONOS devices.

Reduction of Defects on Microstructure Aluminium Nitride Using High Temperature Annealing Heat Treatment

NASA Astrophysics Data System (ADS)

Tanasta, Z.; Muhamad, P.; Kuwano, N.; Norfazrina, H. M. Y.; Unuh, M. H.

2018-03-01

Aluminium Nitride (AlN) is a ceramic 111-nitride material that is used widely as components in functional devices. Besides good thermal conductivity, it also has a high band gap in emitting light which is 6 eV. AlN thin film is grown on the sapphire substrate (0001). However, lattice mismatch between both materials has caused defects to exist along the microstructure of AlN thin films. The defects have affected the properties of Aluminium Nitride. Annealing heat treatment has been proved by the previous researcher to be the best method to improve the microstructure of Aluminium Nitride thin films. Hence, this method is applied at four different temperatures for two hour. The changes of Aluminium Nitride microstructures before and after annealing is observed using Transmission Electron Microscope. It is observed that inversion domains start to occur at temperature of 1500 °C. Convergent Beam Electron Diffraction pattern simulation has confirmed the defects as inversion domain. Therefore, this paper is about to extract the matters occurred during the process of producing high quality Aluminium Nitride thin films and the ways to overcome this problem.

Stressor-layer-induced elastic strain sharing in SrTiO 3 complex oxide sheets

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2018-02-26

A precisely selected elastic strain can be introduced in submicron-thick single-crystal SrTiO 3 sheets using a silicon nitride stressor layer. A conformal stressor layer deposited using plasma-enhanced chemical vapor deposition produces an elastic strain in the sheet consistent with the magnitude of the nitride residual stress. Synchrotron x-ray nanodiffraction reveals that the strain introduced in the SrTiO 3 sheets is on the order of 10 -4, matching the predictions of an elastic model. Using this approach to elastic strain sharing in complex oxides allows the strain to be selected within a wide and continuous range of values, an effect notmore » achievable in heteroepitaxy on rigid substrates.« less

Stressor-layer-induced elastic strain sharing in SrTiO 3 complex oxide sheets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tilka, J. A.; Park, J.; Ahn, Y.

A precisely selected elastic strain can be introduced in submicron-thick single-crystal SrTiO 3 sheets using a silicon nitride stressor layer. A conformal stressor layer deposited using plasma-enhanced chemical vapor deposition produces an elastic strain in the sheet consistent with the magnitude of the nitride residual stress. Synchrotron x-ray nanodiffraction reveals that the strain introduced in the SrTiO 3 sheets is on the order of 10 -4, matching the predictions of an elastic model. Using this approach to elastic strain sharing in complex oxides allows the strain to be selected within a wide and continuous range of values, an effect notmore » achievable in heteroepitaxy on rigid substrates.« less

Piezoelectric Behaviour of Sputtered Aluminium Nitride Thin Film for High Frequency Ultrasonic Sensors

NASA Astrophysics Data System (ADS)

Herzog, T.; Walter, S.; Bartzsch, H.; Gittner, M.; Gloess, D.; Heuer, H.

2011-06-01

Many new materials and processes require non destructive evaluation in higher resolutions by phased array ultrasonic techniques in a frequency range up to 250 MHz. This paper presents aluminium nitride, a promising material for the use as a piezoelectric sensor material in the considered frequency range, which contains the potential for high frequency phased array application in the future. This work represents the fundamental development of piezoelectric aluminium nitride films with a thickness of up to 10 μm. We have investigated and optimized the deposition process of the aluminium nitride thin film layers regarding their piezoelectric behavior. Therefore a specific test setup and a measuring station were created to determine the piezoelectric charge constant (d33) and the electro acoustic behavior of the sensor. Single element transducers were deposited on silicon substrates with aluminium electrodes for top and bottom, using different parameters for the magnetron sputter process, like pressure and bias voltage. Afterwards acoustical measurements up to 500 MHz in pulse echo mode have been carried out and the electrical and electromechanical properties were qualified. In two different parameter sets for the sputtering process excellent piezoelectric charge constant of about 8.0 pC/N maximum were obtained.

Étude par diffraction des rayons X de la nitruration plasma d'un acier 304L Influence sur l'oxydation à 1000 ^{circ}C

NASA Astrophysics Data System (ADS)

Marot, L.; Buscail, H.; Straboni, A.; Riffard, F.; Caudron, E.; Cueff, R.

2002-07-01

This work presents the influence of various nitridation parameters on the 304L steel oxidation at 1000 ^{circ}C, in air under atmospheric pressure. Nitridation temperatures were ranging between 300 ^{circ}C and 430 ^{circ}C with exposure times lasting from 2 to 8 hours. At 300 and 430 ^{circ}C, the nitridation treatment leads to the solid solution surface formation γ-N without any nitride formation. After oxidation at 1000 ^{circ}C of blank specimens, X ray diffraction reveals the FeCr2O4 spinel formation. This oxide does not act as a good diffusion barrier. With nitrogen treated specimens, the higher the nitridation temperature is and the longer the exposure time is, better is the oxidation behaviour at 1000 ^{circ}C. We then observe that the Cr{1,3}Fe{0,7}O3 oxide is more present in the oxide sale from the very beginning of the oxidation test which is correlated to a final lower mass gain. Cette étude porte sur l'influence des paramètres de nitruration plasma sur l'oxydation de l'acier 304L à 1000 ^{circ}C, sous air, à la pression atmosphérique. Les températures employées lors de la nitruration ont été de 300 ^{circ}C et 430 ^{circ}C pour des durées de nitruration variant entre 2 et 8 heures. A 300 et 430 ^{circ}C, la nitruration conduit à la formation d'une solution solide γ-N en surface sans provoquer la formation de nitrures. Après oxydation à 1000 ^{circ}C du 304L non nitruré, la diffraction des rayons X révèle la formation d'une couche de type spinelle FeCr2O4 qui ne semble pas jouer le rôle de barrière de diffusion. Pour les échantillons préalablement nitrurés, plus la température de nitruration est élevée et plus la durée du traitement est longue, meilleur est le comportement en oxydation. Nous observons alors l'oxyde Cr{1,3}Fe{0,7}O3 en proportion importante dès le début de l'oxydation et une prise de masse finale plus faible.

Material impacts and heat flux characterization of an electrothermal plasma source with an applied magnetic field

NASA Astrophysics Data System (ADS)

Gebhart, T. E.; Martinez-Rodriguez, R. A.; Baylor, L. R.; Rapp, J.; Winfrey, A. L.

2017-08-01

To produce a realistic tokamak-like plasma environment in linear plasma device, a transient source is needed to deliver heat and particle fluxes similar to those seen in an edge localized mode (ELM). ELMs in future large tokamaks will deliver heat fluxes of ˜1 GW/m2 to the divertor plasma facing components at a few Hz. An electrothermal plasma source can deliver heat fluxes of this magnitude. These sources operate in an ablative arc regime which is driven by a DC capacitive discharge. An electrothermal source was configured with two pulse lengths and tested under a solenoidal magnetic field to determine the resulting impact on liner ablation, plasma parameters, and delivered heat flux. The arc travels through and ablates a boron nitride liner and strikes a tungsten plate. The tungsten target plate is analyzed for surface damage using a scanning electron microscope.

Preparation of mesoporous carbon nitride structure by the dealloying of Ni/a-CN nanocomposite films

NASA Astrophysics Data System (ADS)

Zhou, Han; Shen, Yongqing; Huang, Jie; Liao, Bin; Wu, Xianying; Zhang, Xu

2018-05-01

The preparation of mesoporous carbon nitride (p-CN) structure by the selective dealloying process of Ni/a-CN nanocomposite films is investigated. The composition and structure of the Ni/a-CN nanocomposite films and porous carbon nitride (p-CN) films are determined by scan electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Phase separated structure including nickel carbide phase and the surrounding amorphous carbon nitride (a-CN) matrix are detected for the as-deposited films. Though the bulk diffusion is introduced in the film during the annealing process, the grain sizes for the post-annealed films are around 10 nm and change little comparing with the ones of the as-deposited films, which is associated with the thermostability of the CN surrounding in the film. The p-CN skeleton with its pore size around 12.5 nm is formed by etching the post-annealed films, indicative of the stability of the phase separated structure during the annealing process.

Preparation of nanocrystalline TiN coated cubic boron nitride powders by a sol-gel process.

PubMed

Park, Hee S; Umer, M Adeel; Ryu, Ho J; Hong, Soon H

2011-01-01

Cubic boron nitride (cBN) particles coated with 20 wt% nanocrystalline TiN were prepared by coating the surface of cBN particles with TiO2, followed by nitridation with NH3 gas at 900 degrees C. Coating of TiO2 on cBN powders was accomplished by a sol-gel process from a solution of titanium (IV) isopropoxide and anhydrous ethanol. An amorphous TiO(x) layer of 50 nm thickness was homogenously formed on the surface of the cBN particles by the sol-gel process. The amorphous layer was then crystallized to an anatase TiO2 phase through calcination in air at 400 degrees C. The crystallized TiO2 layer was 50 nm in thickness, and the size of TiO2 particles comprising the layer was nearly 10 nm. The TiO2 on cBN surfaces was completely converted into nanocrystalline TiN of uniform particles 20 nm in size on cBN particles by nitridation under flowing NH3 gas.

Process for producing high purity silicon nitride by the direct reaction between elemental silicon and nitrogen-hydrogen liquid reactants

DOEpatents

Pugar, Eloise A.; Morgan, Peter E. D.

1990-01-01

A process is disclosed for producing, at a low temperature, a high purity reaction product consisting essentially of silicon, nitrogen, and hydrogen which can then be heated to produce a high purity alpha silicon nitride. The process comprises: reacting together a particulate elemental high purity silicon with a high purity nitrogen-hydrogen reactant in its liquid state (such as ammonia or hydrazine) having the formula: N.sub.n H.sub.(n+m) wherein: n=1-4 and m=2 when the nitrogen-hydrogen reactant is straight chain, and 0 when the nitrogen-hydrogen reactant is cyclic. High purity silicon nitride can be formed from this intermediate product by heating the intermediate product at a temperature of from about 1200.degree.-1700.degree. C. for a period from about 15 minutes up to about 2 hours to form a high purity alpha silicon nitride product. The discovery of the existence of a soluble Si-N-H intermediate enables chemical pathways to be explored previously unavailable in conventional solid state approaches to silicon-nitrogen ceramics.

Process for producing high purity silicon nitride by the direct reaction between elemental silicon and nitrogen-hydrogen liquid reactants

DOEpatents

Pugar, E.A.; Morgan, P.E.D.

1987-09-15

A process is disclosed for producing, at a low temperature, a high purity reaction product consisting essentially of silicon, nitrogen, and hydrogen which can then be heated to produce a high purity alpha silicon nitride. The process comprises: reacting together a particulate elemental high purity silicon with a high purity nitrogen-hydrogen reactant in its liquid state (such as ammonia or hydrazine) having the formula: N/sub n/H/sub (n+m)/ wherein: n = 1--4 and m = 2 when the nitrogen-hydrogen reactant is straight chain, and 0 when the nitrogen-hydrogen reactant is cyclic. High purity silicon nitride can be formed from this intermediate product by heating the intermediate product at a temperature of from about 1200--1700/degree/C for a period from about 15 minutes up to about 2 hours to form a high purity alpha silicon nitride product. The discovery of the existence of a soluble Si/endash/N/endash/H intermediate enables chemical pathways to be explored previously unavailable in conventional solid-state approaches to silicon-nitrogen ceramics

Optimization of process parameters for RF sputter deposition of tin-nitride thin-films

NASA Astrophysics Data System (ADS)

Jangid, Teena; Rao, G. Mohan

2018-05-01

Radio frequency Magnetron sputtering technique was employed to deposit Tin-nitride thin films on Si and glass substrate at different process parameters. Influence of varying parameters like substrate temperature, target-substrate distance and RF power is studied in detail. X-ray diffraction method is used as a key technique for analyzing the changes in the stoichiometric and structural properties of the deposited films. Depending on the combination of deposition parameters, crystalline as well as amorphous films were obtained. Pure tin-nitride thin films were deposited at 15W RF power and 600°C substrate temperature with target-substrate distance fixed at 10cm. Bandgap value of 1.6 eV calculated for the film deposited at optimum process conditions matches well with reported values.

Remarkable biocompatibility enhancement of porous NiTi alloys by a new surface modification approach: in-situ nitriding and in vitro and in vivo evaluation.

PubMed

Li, H; Yuan, B; Gao, Y; Chung, C Y; Zhu, M

2011-12-15

An in-situ nitriding method has been developed to modify the outer surface and the pore walls of both open and closed pores of porous NiTi shape memory alloys (SMAs) as part of their sintering process. XRD and XPS examinations revealed that the modified layer is mainly TiN. The biocompatibility of the in-situ nitrided sample has been characterized by its corrosion resistance, cell adherence, and implant surgery. The in-situ nitrided porous NiTi SMAs exhibit much better corrosion resistance, cell adherence, and bone tissue induced capability than the porous NiTi alloys without surface modification. Furthermore, the released Ni ion content in the blood of rabbit is reduced greatly by the in-situ nitriding. The excellent biocompatibility of in-situ nitrided sample is attributed to the formation of the TiN layer on all the pore walls including both open and closed pores. Copyright © 2011 Wiley Periodicals, Inc.

Functional carbon nitride materials — design strategies for electrochemical devices

NASA Astrophysics Data System (ADS)

Kessler, Fabian K.; Zheng, Yun; Schwarz, Dana; Merschjann, Christoph; Schnick, Wolfgang; Wang, Xinchen; Bojdys, Michael J.

2017-06-01

In the past decade, research in the field of artificial photosynthesis has shifted from simple, inorganic semiconductors to more abundant, polymeric materials. For example, polymeric carbon nitrides have emerged as promising materials for metal-free semiconductors and metal-free photocatalysts. Polymeric carbon nitride (melon) and related carbon nitride materials are desirable alternatives to industrially used catalysts because they are easily synthesized from abundant and inexpensive starting materials. Furthermore, these materials are chemically benign because they do not contain heavy metal ions, thereby facilitating handling and disposal. In this Review, we discuss the building blocks of carbon nitride materials and examine how strategies in synthesis, templating and post-processing translate from the molecular level to macroscopic properties, such as optical and electronic bandgap. Applications of carbon nitride materials in bulk heterojunctions, laser-patterned memory devices and energy storage devices indicate that photocatalytic overall water splitting on an industrial scale may be realized in the near future and reveal a new avenue of 'post-silicon electronics'.

Boron Nitride Nanotubes

NASA Technical Reports Server (NTRS)

Jordan, Kevin (Inventor); Smith, Michael W. (Inventor); Park, Cheol (Inventor)

2012-01-01

Boron nitride nanotubes are prepared by a process which includes: (a) creating a source of boron vapor; (b) mixing the boron vapor with nitrogen gas so that a mixture of boron vapor and nitrogen gas is present at a nucleation site, which is a surface, the nitrogen gas being provided at a pressure elevated above atmospheric, e.g., from greater than about 2 atmospheres up to about 250 atmospheres; and (c) harvesting boron nitride nanotubes, which are formed at the nucleation site.

Development of a Photoelectrochemical Etch Process to Enable Heterogeneous Substrate Integration of Epitaxial III-Nitride Semiconductors

DTIC Science & Technology

2017-12-01

Chung, Stephen Kelley, Kimberley Olver, Blair C. Connelly, Anand V. Sampath, and Meredith L. Reed Sensors and Electron Devices Directorate, ARL...nitride [GaN], indium nitride, and corresponding ternary alloys) provide a basis for a variety of electronic and photonic devices across several...and driven by an electron beam irradiation, which leads to high carrier densities. This necessitates the transfer/removal of the GaN substrate (or GaN

Boron nitride nanotubes

DOEpatents

Smith, Michael W [Newport News, VA; Jordan, Kevin [Newport News, VA; Park, Cheol [Yorktown, VA

2012-06-06

Boron nitride nanotubes are prepared by a process which includes: (a) creating a source of boron vapor; (b) mixing the boron vapor with nitrogen gas so that a mixture of boron vapor and nitrogen gas is present at a nucleation site, which is a surface, the nitrogen gas being provided at a pressure elevated above atmospheric, e.g., from greater than about 2 atmospheres up to about 250 atmospheres; and (c) harvesting boron nitride nanotubes, which are formed at the nucleation site.

Process for manufacture of semipermeable silicon nitride membranes

DOEpatents

Galambos, Paul Charles; Shul, Randy J.; Willison, Christi Gober

2003-12-09

A new class of semipermeable membranes, and techniques for their fabrication, have been developed. These membranes, formed by appropriate etching of a deposited silicon nitride layer, are robust, easily manufacturable, and compatible with a wide range of silicon micromachining techniques.

Shear-Assisted Production of Few-Layer Boron Nitride Nanosheets by Supercritical CO2 Exfoliation and Its Use for Thermally Conductive Epoxy Composites.

PubMed

Tian, Xiaojuan; Li, Yun; Chen, Zhuo; Li, Qi; Hou, Liqiang; Wu, Jiaye; Tang, Yushu; Li, Yongfeng

2017-12-19

Boron nitride nanosheets (BNNS) hold the similar two-dimensional structure as graphene and unique properties complementary to graphene, which makes it attractive in application ranging from electronics to energy storage. The exfoliation of boron nitride (BN) still remains challenge and hinders the applications of BNNS. In this work, the preparation of BNNS has been realized by a shear-assisted supercritical CO 2 exfoliation process, during which supercritical CO 2 intercalates and diffuses between boron nitride layers, and then the exfoliation of BN layers is obtained in the rapid depressurization process by overcoming the van der Waals forces. Our results indicate that the bulk boron nitride has been successfully exfoliated into thin nanosheets with an average 6 layers. It is found that the produced BNNS is well-dispersed in isopropyl alcohol (IPA) with a higher extinction coefficient compared with the bulk BN. Moreover, the BNNS/epoxy composite used as thermal interface materials has been prepared. The introduction of BNNS results in a 313% enhancement in thermal conductivity. Our results demonstrate that BNNS produced by supercritical CO 2 exfoliation show great potential applications for heat dissipation of high efficiency electronics.

Effect of assistant rf field on phase composition of iron nitride film prepared by magnetron sputtering process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, W.L.; Zheng, F.; Fei, W.D.

2006-01-15

Fe-N thin films were fabricated using a direct current magnetron sputtering process assisted by a radio-frequency (rf) field. The effect of the rf field on the phase composition of the films was investigated. The results indicate that with the assistance of the rf field, various kinds of iron nitrides can be obtained in the films, including {alpha}{sup '}-Fe-N, {alpha}{sup ''}-Fe{sub 16}N{sub 2}, {xi}-Fe{sub 2}N, {epsilon}-Fe{sub 3}N, and {gamma}{sup ''}-FeN with ZnS structure. It was found that the rf field greatly benefits the formation of iron nitrides in the Fe-N films.

Effects of Plasma ZrN Metallurgy and Shot Peening Duplex Treatment on Fretting Wear and Fretting Fatigue Behavior of Ti6Al4V Alloy.

PubMed

Tang, Jingang; Liu, Daoxin; Zhang, Xiaohua; Du, Dongxing; Yu, Shouming

2016-03-23

A metallurgical zirconium nitride (ZrN) layer was fabricated using glow metallurgy using nitriding with zirconiuming prior treatment of the Ti6Al4V alloy. The microstructure, composition and microhardness of the corresponding layer were studied. The influence of this treatment on fretting wear (FW) and fretting fatigue (FF) behavior of the Ti6Al4V alloy was studied. The composite layer consisted of an 8-μm-thick ZrN compound layer and a 50-μm-thick nitrogen-rich Zr-Ti solid solution layer. The surface microhardness of the composite layer is 1775 HK 0.1 . A gradient in cross-sectional microhardness distribution exists in the layer. The plasma ZrN metallurgical layer improves the FW resistance of the Ti6Al4V alloy, but reduces the base FF resistance. This occurs because the improvement in surface hardness results in lowering of the toughness and increasing in the notch sensitivity. Compared with shot peening treatment, plasma ZrN metallurgy and shot peening composite treatment improves the FW resistance and enhances the FF resistance of the Ti6Al4V alloy. This is attributed to the introduction of a compressive stress field. The combination of toughness, strength, FW resistance and fatigue resistance enhance the FF resistance for titanium alloy.

Effects of Plasma ZrN Metallurgy and Shot Peening Duplex Treatment on Fretting Wear and Fretting Fatigue Behavior of Ti6Al4V Alloy

PubMed Central

Tang, Jingang; Liu, Daoxin; Zhang, Xiaohua; Du, Dongxing; Yu, Shouming

2016-01-01

A metallurgical zirconium nitride (ZrN) layer was fabricated using glow metallurgy using nitriding with zirconiuming prior treatment of the Ti6Al4V alloy. The microstructure, composition and microhardness of the corresponding layer were studied. The influence of this treatment on fretting wear (FW) and fretting fatigue (FF) behavior of the Ti6Al4V alloy was studied. The composite layer consisted of an 8-μm-thick ZrN compound layer and a 50-μm-thick nitrogen-rich Zr–Ti solid solution layer. The surface microhardness of the composite layer is 1775 HK0.1. A gradient in cross-sectional microhardness distribution exists in the layer. The plasma ZrN metallurgical layer improves the FW resistance of the Ti6Al4V alloy, but reduces the base FF resistance. This occurs because the improvement in surface hardness results in lowering of the toughness and increasing in the notch sensitivity. Compared with shot peening treatment, plasma ZrN metallurgy and shot peening composite treatment improves the FW resistance and enhances the FF resistance of the Ti6Al4V alloy. This is attributed to the introduction of a compressive stress field. The combination of toughness, strength, FW resistance and fatigue resistance enhance the FF resistance for titanium alloy. PMID:28773345

Precursors in the preparation of transition metal nitrides and transition metal carbonitrides and their reaction intermediates

DOEpatents

Maya, Leon

1991-01-01

A process for making ammonolytic precursors to nitride and carbonitride ceramics. Extreme reaction conditions are not required and the precursor is a powder-like substance that produces ceramics of improved purity and morphology upon pyrolysis.

Rear-Sided Passivation by SiNx:H Dielectric Layer for Improved Si/PEDOT:PSS Hybrid Heterojunction Solar Cells.

PubMed

Sun, Yiling; Gao, Pingqi; He, Jian; Zhou, Suqiong; Ying, Zhiqin; Yang, Xi; Xiang, Yong; Ye, Jichun

2016-12-01

Silicon/organic hybrid solar cells have recently attracted great attention because they combine the advantages of silicon (Si) and the organic cells. In this study, we added a patterned passivation layer of silicon nitride (SiNx:H) onto the rear surface of the Si substrate in a Si/poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) ( PSS) hybrid solar cell, enabling an improvement of 0.6 % in the power conversion efficiency (PCE). The addition of the SiNx:H layer boosted the open circuit voltage (V oc) from 0.523 to 0.557 V, suggesting the well-passivation property of the patterned SiNx:H thin layer that was created by plasma-enhanced chemical vapor deposition and lithography processes. The passivation properties that stemmed from front PSS, rear-SiNx:H, front PSS/rear-SiNx:H, etc. are thoroughly investigated, in consideration of the process-related variations.

Deformation-Induced Dissolution and Precipitation of Nitrides in Austenite and Ferrite of a High-Nitrogen Stainless Steel

NASA Astrophysics Data System (ADS)

Shabashov, V. A.; Makarov, A. V.; Kozlov, K. A.; Sagaradze, V. V.; Zamatovskii, A. E.; Volkova, E. G.; Luchko, S. N.

2018-02-01

Methods of Mössbauer spectroscopy and electron microscopy have been used to study the effect of the severe plastic deformation by high pressure torsion in Bridgman anvils on the dissolution and precipitation of chromium nitrides in the austenitic and ferritic structure of an Fe71.2Cr22.7Mn1.3N4.8 high-nitrogen steel. It has been found that an alternative process of dynamic aging with the formation of secondary nitrides affects the kinetics of the dissolution of chromium nitrides. The dynamic aging of ferrite is activated with an increase in the deformation temperature from 80 to 573 K.

Stability and rheology of dispersions of silicon nitride and silicon carbide

NASA Technical Reports Server (NTRS)

Feke, Donald L.

1987-01-01

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.

Development of a Nitride Dispersion Strengthened (NDS) Metallic Alloy for High-Temperature Recuperators

DTIC Science & Technology

1985-06-01

Alloy 2- 40 2-17 Summary of Tensile and Creep/Rupture Results on 0.010-in.-Thick NDS 200 Material 2-41 2-18 Brazing Alloy Screening Tests on NOS 300 2-44...Nitride Strengthening Process 100 - - 90 - __ __ __ __ - 80 __ AFTER NITRIDE AND DENITRIDE CYCLE S 60 - - -- C,50- _ - 40 . 0 200 400 600 800 1000 1200...commercially with development of the 200-series stainless steels and the Nitronic alloys (Armco Steel designation). Manganese also is known to

Fabrication of turbine components and properties of sintered silicon nitride

NASA Technical Reports Server (NTRS)

Neil, J. T.; French, K. W.; Quackenbush, C. L.; Smith, J. T.

1982-01-01

This paper presents a status report on the injection molding of sinterable silicon nitride at GTE Laboratories. The effort involves fabrication of single axial turbine blades and monolithic radial turbine rotors. The injection molding process is reviewed and the fabrication of the turbine components discussed. Oxidation resistance and strength results of current injection molded sintered silicon nitride as well as dimensional checks on sintered turbine blades demonstrate that this material is a viable candidate for high temperature structural applications.

High strength particulate ceramics

DOEpatents

Liles, Kenneth J.; Hoyer, Jesse L.; Mlynarski, Kenneth W.

1991-01-01

This invention relates to new and useful hard, dense, composite materials made from metallic nitrides such as titanium nitride when combined with aluminum oxide and aluminum nitride and a process comprising the steps of: (1) mixing constituent materials using kerosene as a mixing medium; (2) screening, settling, filtering, and washing the mixture in acetone; (3) filling and sealing said materials in a latex mold; (4) isostatically pressing the material into a compacted powder; and (5) sintering the compacted powder in a gas atmosphere at 1,850.degree. C. for two hours.

Conformal chemically resistant coatings for microflow devices

DOEpatents

Folta, James A.; Zdeblick, Mark

2003-05-13

A process for coating the inside surfaces of silicon microflow devices, such as electrophoresis microchannels, with a low-stress, conformal (uniform) silicon nitride film which has the ability to uniformly coat deeply-recessed cavities with, for example, aspect ratios of up to 40:1 or higher. The silicon nitride coating allows extended exposure to caustic solutions. The coating enables a microflow device fabricated in silicon to be resistant to all classes of chemicals: acids, bases, and solvents. The process involves low-pressure (vacuum) chemical vapor deposition. The ultra-low-stress silicon nitride deposition process allows 1-2 .mu.m thick films without cracks, and so enables extended chemical protection of a silicon microflow device against caustics for up to 1 year. Tests have demonstrated the resistance of the films to caustic solutions at both ambient and elevated temperatures to 65.degree. C.

Aspects of the practical application of titanium alloys after low temperature nitriding glow discharge in hydrogen- free -gas media

NASA Astrophysics Data System (ADS)

Mashovets, N. S.; Pastukh, I. M.; Voloshko, S. M.

2017-01-01

X-ray diffraction analysis, X-ray photoelectron spectroscopy, and Electron Auger-spectroscopy investigation of phase transformation on the surface of the VT8 titanium alloy after a low temperature hydrogen-free nitriding in a glow discharge. Operational characteristics of titanium alloys defined physical-mechanical characteristics of the surface and their phase composition, which depend on the process parameters of nitriding. Surface modification of titanium alloys were carried out by low-temperature nitriding in a glow discharge in hydrogen-free environment. The main advantage of this method lies in the absence of hydrogen embrittlement and complete environmental safety process. Application of the glow discharge can not only speed up the process by the order of the diffusion surface saturation with nitrogen, but also significantly alters the kinetics of the process and quality of the nitrided layer, in particular its physio-mechanical properties and phase composition. For research purposes, the standards from an α + β alloy Ti-Al6-Cr2-Mo2,5 (VT8) were used. Research into the phase composition was performed by X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). Stratified analysis by AES was conducted by etching the surface of the samples' argon ion beam with diameters of 1.5 mm with an energy of 3000 eV and a current density of 400 mA/cm2. The above material shows the promise of the technology of low-temperature hydrogen-nitriding by glow discharge. This greatly expands the range of practical applications of titanium alloys. In addition, changing the technological mode allows you to manage a wide range of modified phase composition of the surface layer and as a result - to form the surface of titanium parts, taking into account the conditions of the subsequent operation.

Powder Injection Molding of Ceramic Engine Components for Transportation

NASA Astrophysics Data System (ADS)

Lenz, Juergen; Enneti, Ravi K.; Onbattuvelli, Valmikanathan; Kate, Kunal; Martin, Renee; Atre, Sundar

2012-03-01

Silicon nitride has been the favored material for manufacturing high-efficiency engine components for transportation due to its high temperature stability, good wear resistance, excellent corrosion resistance, thermal shock resistance, and low density. The use of silicon nitride in engine components greatly depends on the ability to fabricate near net-shape components economically. The absence of a material database for design and simulation has further restricted the engineering community in developing parts from silicon nitride. In this paper, the design and manufacturability of silicon nitride engine rotors for unmanned aerial vehicles by the injection molding process are discussed. The feedstock material property data obtained from experiments were used to simulate the flow of the material during injection molding. The areas susceptible to the formation of defects during the injection molding process of the engine component were identified from the simulations. A test sample was successfully injection molded using the feedstock and sintered to 99% density without formation of significant observable defects.

Dissolution and Characterization of Boron Nitride Nanotubes in Superacid.

PubMed

Kleinerman, Olga; Adnan, Mohammed; Marincel, Daniel M; Ma, Anson W K; Bengio, E Amram; Park, Cheol; Chu, Sang-Hyon; Pasquali, Matteo; Talmon, Yeshayahu

2017-12-19

Boron nitride nanotubes (BNNTs) are of interest for their unique combination of high tensile strength, high electrical resistivity, high neutron cross section, and low reactivity. The fastest route to employing these properties in composites and macroscopic articles is through solution processing. However, dispersing BNNTs without functionalization or use of a surfactant is challenging. We show here by cryogenic transmission electron microscopy that BNNTs spontaneously dissolve in chlorosulfonic acid as disentangled individual molecules. Electron energy loss spectroscopy of BNNTs dried from the solution confirms preservation of the sp 2 hybridization for boron and nitrogen, eliminating the possibility of BNNT functionalization or damage. The length and diameter of the BNNTs was statistically calculated to be ∼4.5 μm and ∼4 nm, respectively. Interestingly, bent or otherwise damaged BNNTs are filled by chlorosulfonic acid. Additionally, nanometer-sized synthesis byproducts, including boron nitride clusters, isolated single and multilayer hexagonal boron nitride, and boron particles, were identified. Dissolution in superacid provides a route for solution processing BNNTs without altering their chemical structure.

Solid solution lithium alloy cermet anodes

DOEpatents

Richardson, Thomas J.

2013-07-09

A metal-ceramic composite ("cermet") has been produced by a chemical reaction between a lithium compound and another metal. The cermet has advantageous physical properties, high surface area relative to lithium metal or its alloys, and is easily formed into a desired shape. An example is the formation of a lithium-magnesium nitride cermet by reaction of lithium nitride with magnesium. The reaction results in magnesium nitride grains coated with a layer of lithium. The nitride is inert when used in a battery. It supports the metal in a high surface area form, while stabilizing the electrode with respect to dendrite formation. By using an excess of magnesium metal in the reaction process, a cermet of magnesium nitride is produced, coated with a lithium-magnesium alloy of any desired composition. This alloy inhibits dendrite formation by causing lithium deposited on its surface to diffuse under a chemical potential into the bulk of the alloy.

Distribution of nitrogen and defects in SiO(x)N(y)/Si structures formed by the thermal nitridation of SiO2/Si

NASA Technical Reports Server (NTRS)

Vasquez, R. P.; Madhukar, A.; Grunthaner, F. J.; Naiman, M. L.

1986-01-01

Previously reported nitrogen distributions in SiO2 films on Si which have been thermally nitrided at 1000 C have been explained by a kinetic model of the nitridation process which rests upon the effects of interfacial strain. A critical test of this kinetic model is the validity of the predictions regarding nitrogen distributions obtained at other nitridation temperatures. In this work, nitrogen distributions determined via X-ray photoelectron spectroscopy are reported for samples nitrided at 800 and 1150 C, and are shown to be consistent with the kinetic model. In addition, the intensity of a fluorine marker is found to correlate with the nitrogen distribution, and is postulated to be related to kinetically generated defects in the dielectric film, consistent with the strain-dependent energy of formation of defects proposed recently to explain electrical data.

Gradient microstructure and microhardness in a nitrided 18CrNiMo7-6 gear steel

NASA Astrophysics Data System (ADS)

Yang, R.; Wu, G. L.; Zhang, X.; Fu, W. T.; Huang, X.

2017-07-01

A commercial gear steel (18CrNiMo7-6) containing a tempered martensite structure was nitrided using a pressurized gas nitriding process under a pressure of 5 atm at 530 °C for 5 hours. The mechanical properties and microstructure of the nitrided sample were characterized by Vickers hardness measurements, X-ray diffraction, and backscatter electron imaging in a scanning electron microscope. A micro-hardness gradient was identified over a distance of 500 μm with hardness values of 900 HV at the top surface and 300 HV in the core. This micro-hardness gradient corresponds to a gradient in the microstructure that changes from a nitride compound layer at the top surface (∼ 20 μm thick) to a diffusion zone with a decreasing nitrogen concentration and precipitate density with distance from the surface, finally reaching the core matrix layer with a recovered martensite structure.

Room-Temperature Synthesis of GaN Driven by Kinetic Energy beyond the Limit of Thermodynamics.

PubMed

Imaoka, Takane; Okada, Takeru; Samukawa, Seiji; Yamamoto, Kimihisa

2017-12-06

The nitridation reaction is significantly important to utilize the unique properties of nitrides and nitrogen-doped materials. However, nitridation generally requires a high temperature or highly reactive reagents (often explosive) because the energies of N-N bond cleavage and nitrogen anion formation (N 3- ) are very high. We demonstrate the first room-temperature synthesis of GaN directly from GaCl 3 by nanoscale atom exchange reaction. Nonequilibrium nitrogen molecules with very high translational energy were used as a chemically stable and safe nitrogen source. The irradiation of molecular nitrogen to the desired reaction area successfully provided a gallium nitride (GaN) nanosheet that exhibited a typical photoluminescence spectrum. Because this process retains the target substrate room temperature and does not involve any photon nor charged ion, it allows damage-less synthesis of the semiconducting metal nitrides, even directly on plastic substrates such as polyethylene terephthalate (PET).

An investigation of nitride precipitates in archaeological iron artefacts from Poland.

PubMed

Kedzierski, Z; Stepiński, J; Zielińska-Lipiec, A

2010-03-01

The paper describes the investigations of nitride precipitates in a spearhead and a sword found in the territory of Poland, in cremation graveyards of the Przeworsk Culture, dated to the Roman Period. Three different techniques of the examination of nitride precipitates were employed: optical microscope, scanning electron microscope (scanning electron microscope with energy dispersive X-ray spectrometer) and transmission electron microscope. Two types of precipitates have been observed, and their plate-like shape was demonstrated. The large precipitate has been confirmed to be gamma'-Fe(4)N, whereas the small one has been identified as alpha''-Fe(16)N(2). The origin of nitride precipitates in archaeological iron artefacts from Poland is probably a result of the manufacturing process or cremation as part of burial rites. An examination of available iron artefacts indicates that nitride precipitates (have only limited effect on mechanical properties) influence the hardness of metal only to a very limited degree.

Study of phenomena related to the sintering process of silicon nitride at atmospheric pressure

NASA Technical Reports Server (NTRS)

Bertani, A.

1982-01-01

A procedure was perfected for the production of components used in engineering applications of silicon nitride. Particles of complex geometry that combine remarkable mechanical properties with a high density are obtained. The process developed, in contrast to the "hot pressing" method, does not use external pressures, and in contrast to the reaction bonding method, final densities close to the theoretical value are obtained.

Doping of free-standing zinc-blende GaN layers grown by molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Novikov, S. V.; Powell, R. E. L.; Staddon, C. R.; Kent, A. J.; Foxon, C. T.

2014-10-01

Currently there is high level of interest in developing of vertical device structures based on the group III nitrides. We have studied n- and p-doping of free-standing zinc-blende GaN grown by plasma-assisted molecular beam epitaxy (PA-MBE). Si was used as the n-dopant and Mg as the p-dopant for zinc-blende GaN. Controllable levels of doping with Si and Mg in free-standing zinc-blende GaN have been achieved by PA-MBE. The Si and Mg doping depth uniformity through the zinc-blende GaN layers have been confirmed by secondary ion mass spectrometry (SIMS). Controllable Si and Mg doping makes PA-MBE a promising method for the growth of conducting group III-nitrides bulk crystals.

Hexagonal Ag nanoarrays induced enhancement of blue light emission from amorphous oxidized silicon nitride via localized surface plasmon coupling.

PubMed

Ma, Zhongyuan; Ni, Xiaodong; Zhang, Wenping; Jiang, Xiaofan; Yang, Huafeng; Yu, Jie; Wang, Wen; Xu, Ling; Xu, Jun; Chen, Kunji; Feng, Duan

2014-11-17

A significant enhancement of blue light emission from amorphous oxidized silicon nitride (a-SiNx:O) films is achieved by introduction of ordered and size-controllable arrays of Ag nanoparticles between the silicon substrate and a-SiNx:O films. Using hexagonal arrays of Ag nanoparticles fabricated by nanosphere lithography, the localized surface plasmons (LSPs) resonance can effectively increase the internal quantum efficiency from 3.9% to 13.3%. Theoretical calculation confirms that the electromagnetic field-intensity enhancement is through the dipole surface plasma coupling with the excitons of a-SiNx:O films, which demonstrates a-SiNx:O films with enhanced blue emission are promising for silicon-based light-emitting applications by patterned Ag arrays.

Investigating plasma viscosity with fast framing photography in the ZaP-HD Flow Z-Pinch experiment

NASA Astrophysics Data System (ADS)

Weed, Jonathan Robert

The ZaP-HD Flow Z-Pinch experiment investigates the stabilizing effect of sheared axial flows while scaling toward a high-energy-density laboratory plasma (HEDLP > 100 GPa). Stabilizing flows may persist until viscous forces dissipate a sheared flow profile. Plasma viscosity is investigated by measuring scale lengths in turbulence intentionally introduced in the plasma flow. A boron nitride turbulence-tripping probe excites small scale length turbulence in the plasma, and fast framing optical cameras are used to study time-evolved turbulent structures and viscous dissipation. A Hadland Imacon 790 fast framing camera is modified for digital image capture, but features insufficient resolution to study turbulent structures. A Shimadzu HPV-X camera captures the evolution of turbulent structures with great spatial and temporal resolution, but is unable to resolve the anticipated Kolmogorov scale in ZaP-HD as predicted by a simplified pinch model.

Performance, Stability, and Plume Characterization of the HERMeS Thruster with Boron Nitride Silica Composite Discharge Channel

NASA Technical Reports Server (NTRS)

Kamhawi, Hani; Huang, Wensheng; Gilland, James H.; Haag, Thomas W.; Mackey, Jonathan; Yim, John; Pinero, Luis; Williams, George; Peterson, Peter; Herman, Daniel

2017-01-01

NASA's Hall Effect Rocket with Magnetic Shielding (HERMeS) 12.5kW Technology Demonstration Unit-3 (TDU-3) has been the subject of extensive technology maturation in preparation for flight system development. Detailed performance, stability, and plume characterization tests of the thruster were performed at NASA GRC's Vacuum Facility 5 (VF-5). The TDU-3 thruster implements a magnetic topology that is identical to TDU-1. The TDU-3 boron nitride silica composite discharge channel material is different than the TDU-1 heritage boron nitride discharge channel material. Performance and stability characterization of the TDU-3 thruster was performed at discharge voltages between 300V and 600V and at discharge currents between 5A and 21.8A. The thruster performance and stability were assessed for varying magnetic field strength, cathode flow fractions between 5% and 9%, varying harness inductance, and for reverse magnet polarity. Performance characterization test results indicate that the TDU-3 thruster performance is in family with the TDU-1 levels. TDU-3's thrust efficiency of 65% and specific impulse of 2,800sec at 600V and 12.5kW exceed performance levels of SOA Hall thrusters. Thruster stability regimes were characterized with respect to the thruster discharge current oscillations (discharge current peak-to-peak and root mean square magnitudes), discharge current waveform power spectral density analysis, and maps of the current-voltage-magnetic field. Stability characterization test results indicate a stability profile similar to TDU-1. Finally, comparison of the TDU-1 and TDU-3 plume profiles found that there were negligible differences in the plasma plume characteristics between the TDU with heritage boron nitride versus the boron nitride silica composite discharge channel.

Formation process and mechanism of iron-nitride compounds on Si(1 1 1)-7 × 7-CH3OH surface

NASA Astrophysics Data System (ADS)

Li, Wenxin; Ding, Wanyu; Ju, Dongying; Tanaka, Ken-ichi; Komori, Fumio

2018-07-01

Fe atoms were deposited on Si(1 1 1)-7 × 7 restructured surface, which had been covered by CH3OH molecules. A newly formed surface is stabilized by a quasi-potential made by breaking, and adsorbed atoms or molecules can be stabilized by forming "quasi-compounds". Then, aim to greatly enhance the magnetic properties of the memory units, nitriding experiments were implemented on the existing Fe compounds. With the in-situ observation of STM, a series of Fe3N structures make up the newly emerged iron-nitride compounds, showing good linear characteristics. By adjusting the concentration, this study further explored its formation process and compounds models.

Formation of porous surface layers in reaction bonded silicon nitride during processing

NASA Technical Reports Server (NTRS)

Shaw, N. J.; Glasgow, T. K.

1979-01-01

Microstructural examination of reaction bonded silicon nitride (RBSN) has shown that there is often a region adjacent to the as-nitrided surfaces that is even more porous than the interior of this already quite porous material. Because this layer of large porosity is considered detrimental to both the strength and oxidation resistance of RBSN, a study was undertaken to determine if its formation could be prevented during processing. All test bars studied were made from a single batch of Si powder which was milled for 4 hours in heptane in a vibratory mill using high density alumina cylinders as the grinding media. After air drying the powder, bars were compacted in a single acting die and hydropressed.

Substrate nitridation induced modulations in transport properties of wurtzite GaN/p-Si (100) heterojunctions grown by molecular beam epitaxy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhat, Thirumaleshwara N.; Rajpalke, Mohana K.; Krupanidhi, S. B.

Phase pure wurtzite GaN films were grown on Si (100) substrates by introducing a silicon nitride layer followed by low temperature GaN growth as buffer layers. GaN films grown directly on Si (100) were found to be phase mixtured, containing both cubic ({beta}) and hexagonal ({alpha}) modifications. The x-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence (PL) spectroscopy studies reveal that the significant enhancement in the structural as well as in the optical properties of GaN films grown with silicon nitride buffer layer grown at 800 deg. C when compared to the samples grown in the absence of silicon nitridemore » buffer layer and with silicon nitride buffer layer grown at 600 deg. C. Core-level photoelectron spectroscopy of Si{sub x}N{sub y} layers reveals the sources for superior qualities of GaN epilayers grown with the high temperature substrate nitridation process. The discussion has been carried out on the typical inverted rectification behavior exhibited by n-GaN/p-Si heterojunctions. Considerable modulation in the transport mechanism was observed with the nitridation conditions. The heterojunction fabricated with the sample of substrate nitridation at high temperature exhibited superior rectifying nature with reduced trap concentrations. Lowest ideality factors ({approx}1.5) were observed in the heterojunctions grown with high temperature substrate nitridation which is attributed to the recombination tunneling at the space charge region transport mechanism at lower voltages and at higher voltages space charge limited current conduction is the dominating transport mechanism. Whereas, thermally generated carrier tunneling and recombination tunneling are the dominating transport mechanisms in the heterojunctions grown without substrate nitridation and low temperature substrate nitridation, respectively.« less

Materials Analysis of Transient Plasma-Wall Interactions

DTIC Science & Technology

2014-05-13

such as copper, aluminum, zirconium, titanium, and tungsten) and ceramics (beryllia, aluminum nitride, silicon carbide , etc.). These materials were...formation of silicon carbide . Therefore, a flat Macor disk was polished, and prepared for deuterium exposure by sonicating the sample in both methanol...of silicon constituents whereas the exposed sample clearly shows the addition of carbide and silicon segregation on the surface. 10 AFOSR

Cytocompatibility of amorphous hydrogenated carbon nitride films deposited by CH4/N2 dielectric barrier discharge plasmas with respect to cell lines

NASA Astrophysics Data System (ADS)

Majumdar, Abhijit; Schröder, Karsten; Hippler, Rainer

2008-10-01

Special amorphous hydrogenated carbon nitride (a-H-CNx) films have been prepared on glass substrates for the investigation of adhesion and proliferation of different mammalian cell lines. CH4/N2 dielectric barrier discharge plasmas were applied to deposit a-H-CNx coatings at half of the atmospheric pressure. Film quality was modified by varying the CH4:N2 ratio and deposition duration. Chemical composition was determined by x-ray photoelectron spectroscopy and Fourier transformed infrared spectroscopy. The N/C ratio was in the range of 0.20-0.55. A very small surface roughness was verified by atomic force microscopy. Human embryonic kidney (HEK) and rat adrenal pheochromocytoma (PC12) cells were cultivated on the a-H-CNx films to investigate the cytocompatibility of these surfaces. The microscopic images show that both kinds of cells lines were unable to survive. The cells did not adhere to the surfaces, and most of the cells died after certain time spans. Increased amounts of nitrogen in the film induce an accelerated cell death. It is concluded, that the deposited CNx film behaves cytotoxic to HEK and PC12 cell lines.

Ferrocene-modified carbon nitride for direct oxidation of benzene to phenol with visible light.

PubMed

Ye, Xiangju; Cui, Yanjuan; Wang, Xinchen

2014-03-01

Ferrocene moieties were heterogenized onto carbon nitride polymers by a covalent -C=N- linkage bridging the two conjugation systems, enabling the merging of the redox function of ferrocene with carbon nitride photocatalysis to construct a heterogeneous Photo-Fenton system for green organocatalysis at neutral conditions. The synergistic donor-acceptor interaction between the carbon nitride matrix and ferrocene group, improved exciton splitting, and coupled photocatalytic performance allowed the direct synthesis of phenol from benzene in the presence of H2 O2 under visible light irradiation. This innovative modification method will offer an avenue to construct functionalized two-dimensional polymers useful also for other green synthesis processes using solar irradiation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Second-harmonic generation in substoichiometric silicon nitride layers

NASA Astrophysics Data System (ADS)

Pecora, Emanuele; Capretti, Antonio; Miano, Giovanni; Dal Negro, Luca

2013-03-01

Harmonic generation in optical circuits offers the possibility to integrate wavelength converters, light amplifiers, lasers, and multiple optical signal processing devices with electronic components. Bulk silicon has a negligible second-order nonlinear optical susceptibility owing to its crystal centrosymmetry. Silicon nitride has its place in the microelectronic industry as an insulator and chemical barrier. In this work, we propose to take advantage of silicon excess in silicon nitride to increase the Second Harmonic Generation (SHG) efficiency. Thin films have been grown by reactive magnetron sputtering and their nonlinear optical properties have been studied by femtosecond pumping over a wide range of excitation wavelengths, silicon nitride stoichiometry and thermal processes. We demonstrate SHG in the visible range (375 - 450 nm) using a tunable 150 fs Ti:sapphire laser, and we optimize the SH emission at a silicon excess of 46 at.% demonstrating a maximum SHG efficiency of 4x10-6 in optimized films. Polarization properties, generation efficiency, and the second order nonlinear optical susceptibility are measured for all the investigated samples and discussed in terms of an effective theoretical model. Our findings show that the large nonlinear optical response demonstrated in optimized Si-rich silicon nitride materials can be utilized for the engineering of nonlinear optical functions and devices on a Si chip.

Use of cermet thin film resistors with nitride passivated metal insulator field effect transistor

NASA Technical Reports Server (NTRS)

Brown, G. A.; Harrap, V.

1971-01-01

Film deposition of cermet resistors on same chip with metal nitride oxide silicon field effect transistors permits protection of contamination sensitive active devices from contaminants produced in cermet deposition and definition processes. Additional advantages include lower cost, greater reliability, and space savings.

Method of preparing uranium nitride or uranium carbonitride bodies

DOEpatents

Wilhelm, Harley A.; McClusky, James K.

1976-04-27

Sintered uranium nitride or uranium carbonitride bodies having a controlled final carbon-to-uranium ratio are prepared, in an essentially continuous process, from U.sub.3 O.sub.8 and carbon by varying the weight ratio of carbon to U.sub.3 O.sub.8 in the feed mixture, which is compressed into a green body and sintered in a continuous heating process under various controlled atmospheric conditions to prepare the sintered bodies.

Theoretical study of the ammonia nitridation rate on an Fe (100) surface: a combined density functional theory and kinetic Monte Carlo study.

PubMed

Yeo, Sang Chul; Lo, Yu Chieh; Li, Ju; Lee, Hyuck Mo

2014-10-07

Ammonia (NH3) nitridation on an Fe surface was studied by combining density functional theory (DFT) and kinetic Monte Carlo (kMC) calculations. A DFT calculation was performed to obtain the energy barriers (Eb) of the relevant elementary processes. The full mechanism of the exact reaction path was divided into five steps (adsorption, dissociation, surface migration, penetration, and diffusion) on an Fe (100) surface pre-covered with nitrogen. The energy barrier (Eb) depended on the N surface coverage. The DFT results were subsequently employed as a database for the kMC simulations. We then evaluated the NH3 nitridation rate on the N pre-covered Fe surface. To determine the conditions necessary for a rapid NH3 nitridation rate, the eight reaction events were considered in the kMC simulations: adsorption, desorption, dissociation, reverse dissociation, surface migration, penetration, reverse penetration, and diffusion. This study provides a real-time-scale simulation of NH3 nitridation influenced by nitrogen surface coverage that allowed us to theoretically determine a nitrogen coverage (0.56 ML) suitable for rapid NH3 nitridation. In this way, we were able to reveal the coverage dependence of the nitridation reaction using the combined DFT and kMC simulations.

Characterizing AISI 1045 steel surface duplex-treated by alternating current field enhanced pack aluminizing and nitriding

NASA Astrophysics Data System (ADS)

Xie, Fei; Zhang, Ge; Pan, Jianwei

2018-02-01

Thin cases and long treating time are shortcomings of conventional duplex treatment of aluminizing followed by nitriding (DTAN). Alternating current field (ACF) enhanced DTAN was carried out on AISI 1045 steel by applying an ACF to treated samples and treating agents with a pair of electrodes for overcoming those shortcomings. By investigating cases' structures, phases, composition and hardness distributions of differently treated samples, preliminary studies were made on characterizations of the ACF enhanced duplex treatment to AISI 1045 steel. The results show that, with the help of the ACF, the surface Al-rich phase Al5Fe2 formed in conventional pack aluminizing can be easily avoided and the aluminizing process is dramatically promoted. The aluminizing case can be nitrided either with conventional pack nitriding or ACF enhanced pack nitriding. By applying ACF to pack nitriding, the diffusion of nitrogen into the aluminizing case is promoted. AlN, Fe2∼3N and solid solution of N in iron are efficiently formed as a result of reactions of N with the aluminizing case. A duplex treated case with an effective thickness of more than 170 μm can be obtained by the alternating current field enhanced 4 h pack aluminizing plus 4 h pack nitriding.

Silicon nitride photonics: from visible to mid-infrared wavelengths

NASA Astrophysics Data System (ADS)

Micó, Gloria; Bru, Luis A.; Pastor, Daniel; Doménech, David; Fernández, Juan; Sánchez, Ana; Cirera, Josep M.; Domínguez, Carlos; Muñoz, Pascual

2018-02-01

Silicon nitride has received a lot of attention during the last ten years, for applications such as bio-photonics, tele/datacom, optical signal processing and sensing. In this paper, firstly an updated review of the state of the art of silicon nitride photonics integration platforms will be provided. Secondly, our developments on a moderate confinement Si3N4 platform in the near-infrared will be presented. Finally, our steps towards establishing a Si3N4 based platform for broadband operation spanning from visible to mid-infrared wavelengths will be introduced.

Polymeric carbon nitride for solar hydrogen production.

PubMed

Li, Xiaobo; Masters, Anthony F; Maschmeyer, Thomas

2017-07-04

If solar hydrogen production from water is to be a realistic candidate for industrial hydrogen production, the development of photocatalysts, which avoid the use of expensive and/or toxic elements is highly desirable from a scalability, cost and environmental perspective. Metal-free polymeric carbon nitride is an attractive material that can absorb visible light and produce hydrogen from water. This article reviews recent developments in polymeric carbon nitride as used in photocatalysis and then develops the discussion focusing on the three primary processes of a photocatalytic reaction: light-harvesting, carrier generation/separation/transportation and surface reactions.

Study of electrochemical properties of thin film materials obtained using plasma technologies for production of electrodes for pacemakers

NASA Astrophysics Data System (ADS)

Obrezkov, O. I.; Vinogradov, V. P.; Krauz, V. I.; Mozgrin, D. V.; Guseva, I. A.; Andreev, E. S.; Zverev, A. A.; Starostin, A. L.

2016-09-01

Studies of thin film materials (TFM) as coatings of tips of pacemaker electrodes implanted into the human heart have been performed. TFM coatings were deposited in vacuum by arc magnetron discharge plasma, by pulsed discharge of “Plasma Focus”, and by electron beam evaporation. Simulation of electric charge transfer to the heart in physiological blood- imitator solution and determination of electrochemical properties of the coatings were carried out. TFM of highly developed surface of contact with tissue was produced by argon plasma spraying of titanium powder with subsequent coating by titanium nitride in vacuum arc assisted by Ti ion implantation. The TFM coatings of pacemaker electrode have passed necessary clinical tests and were used in medical practice. They provide low voltage myocardium stimulation thresholds within the required operating time.

High-density convergent plasma sputtering device for a liquid metal target using an unheated glass plate

NASA Astrophysics Data System (ADS)

Motomura, T.; Tabaru, T.

2018-06-01

A high-density convergent plasma sputtering device has been developed for a liquid metal target, using an unheated glass plate. The convergent magnetic field lines, which are produced by an external solenoid coil and a permanent magnet positioned behind the liquid metal target, effectively transport high-density plasmas near the target. In this study, a liquid gallium target was sputtered with nitrogen plasmas, without additive gas required for depositing gallium nitride films on the unheated substrates. The deposition rate of the GaN film was estimated at ˜13 nm/min at a gas pressure of 0.2 Pa. A strong diffraction peak was observed along the GaN (002) axis, with the use of an unheated glass plate and a target-substrate distance of ˜45 mm.

Energy efficiency in nanoscale synthesis using nanosecond plasmas.

PubMed

Pai, David Z; Ken Ostrikov, Kostya; Kumar, Shailesh; Lacoste, Deanna A; Levchenko, Igor; Laux, Christophe O

2013-01-01

We report a nanoscale synthesis technique using nanosecond-duration plasma discharges. Voltage pulses 12.5 kV in amplitude and 40 ns in duration were applied repetitively at 30 kHz across molybdenum electrodes in open ambient air, generating a nanosecond spark discharge that synthesized well-defined MoO₃ nanoscale architectures (i.e. flakes, dots, walls, porous networks) upon polyamide and copper substrates. No nitrides were formed. The energy cost was as low as 75 eV per atom incorporated into a nanostructure, suggesting a dramatic reduction compared to other techniques using atmospheric pressure plasmas. These findings show that highly efficient synthesis at atmospheric pressure without catalysts or external substrate heating can be achieved in a simple fashion using nanosecond discharges.

Droplet heteroepitaxy of zinc-blende vs. wurtzite GaN quantum dots

NASA Astrophysics Data System (ADS)

Reese, C.; Jeon, S.; Hill, T.; Jones, C.; Shusterman, S.; Yacoby, Y.; Clarke, R.; Deng, H.; Goldman, Rs

We have developed a GaN droplet heteroepitaxy process based upon plasma-assisted molecular-beam epitaxy. Using various surface treatments and Ga deposition parameters, we have demonstrated polycrystalline, zinc-blende (ZB), and wurtzite (WZ) GaN quantum dots (QDs) on Si(001), r-Al2O3, Si(111), and c-GaN substrates. For the polar substrates (i.e. Si(111) and c-GaN), high-resolution transmission electron microscopy and coherent Bragg rod analysis reveals the formation of coherent WZ GaN QDs with nitridation-temperature-dependent sizes and densities. For the non-polar substrates (i.e. Si(001) and r-Al2O3) , QDs with strong near-band photoluminescence emission are observed and ZB GaN QD growth on Si(001) is demonstrated for the first time.

Gallium nitride heterostructures on 3D structured silicon.

PubMed

Fündling, Sönke; Sökmen, Unsal; Peiner, Erwin; Weimann, Thomas; Hinze, Peter; Jahn, Uwe; Trampert, Achim; Riechert, Henning; Bakin, Andrey; Wehmann, Hergo-Heinrich; Waag, Andreas

2008-10-08

We investigated GaN-based heterostructures grown on three-dimensionally patterned Si(111) substrates by metal organic vapour phase epitaxy, with the goal of fabricating well controlled high quality, defect reduced GaN-based nanoLEDs. The high aspect ratios of such pillars minimize the influence of the lattice mismatched substrate and improve the material quality. In contrast to other approaches, we employed deep etched silicon substrates to achieve a controlled pillar growth. For that a special low temperature inductively coupled plasma etching process has been developed. InGaN/GaN multi-quantum-well structures have been incorporated into the pillars. We found a pronounced dependence of the morphology of the GaN structures on the size and pitch of the pillars. Spatially resolved optical properties of the structures are analysed by cathodoluminescence.

Material impacts and heat flux characterization of an electrothermal plasma source with an applied magnetic field

DOE PAGES

Gebhart, T. E.; Martinez-Rodriguez, R. A.; Baylor, L. R.; ...

2017-08-11

To produce a realistic tokamak-like plasma environment in linear plasma device, a transient source is needed to deliver heat and particle fluxes similar to those seen in an edge localized mode (ELM). ELMs in future large tokamaks will deliver heat fluxes of ~1 GW/m 2 to the divertor plasma facing components at a few Hz. An electrothermal plasma source can deliver heat fluxes of this magnitude. These sources operate in an ablative arc regime which is driven by a DC capacitive discharge. An electrothermal source was configured in this paper with two pulse lengths and tested under a solenoidal magneticmore » field to determine the resulting impact on liner ablation, plasma parameters, and delivered heat flux. The arc travels through and ablates a boron nitride liner and strikes a tungsten plate. Finally, the tungsten target plate is analyzed for surface damage using a scanning electron microscope.« less

Material impacts and heat flux characterization of an electrothermal plasma source with an applied magnetic field

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gebhart, T. E.; Martinez-Rodriguez, R. A.; Baylor, L. R.

To produce a realistic tokamak-like plasma environment in linear plasma device, a transient source is needed to deliver heat and particle fluxes similar to those seen in an edge localized mode (ELM). ELMs in future large tokamaks will deliver heat fluxes of ~1 GW/m 2 to the divertor plasma facing components at a few Hz. An electrothermal plasma source can deliver heat fluxes of this magnitude. These sources operate in an ablative arc regime which is driven by a DC capacitive discharge. An electrothermal source was configured in this paper with two pulse lengths and tested under a solenoidal magneticmore » field to determine the resulting impact on liner ablation, plasma parameters, and delivered heat flux. The arc travels through and ablates a boron nitride liner and strikes a tungsten plate. Finally, the tungsten target plate is analyzed for surface damage using a scanning electron microscope.« less

Plasma-assisted Molecular Beam Epitaxy of N-polar InAlN-barrier High-electron-mobility Transistors.

PubMed

Hardy, Matthew T; Storm, David F; Katzer, D Scott; Downey, Brian P; Nepal, Neeraj; Meyer, David J

2016-11-24

Plasma-assisted molecular beam epitaxy is well suited for the epitaxial growth of III-nitride thin films and heterostructures with smooth, abrupt interfaces required for high-quality high-electron-mobility transistors (HEMTs). A procedure is presented for the growth of N-polar InAlN HEMTs, including wafer preparation and growth of buffer layers, the InAlN barrier layer, AlN and GaN interlayers and the GaN channel. Critical issues at each step of the process are identified, such as avoiding Ga accumulation in the GaN buffer, the role of temperature on InAlN compositional homogeneity, and the use of Ga flux during the AlN interlayer and the interrupt prior to GaN channel growth. Compositionally homogeneous N-polar InAlN thin films are demonstrated with surface root-mean-squared roughness as low as 0.19 nm and InAlN-based HEMT structures are reported having mobility as high as 1,750 cm 2 /V∙sec for devices with a sheet charge density of 1.7 x 10 13 cm -2 .

The continued development of the Spallation Neutron Source external antenna H- ion sourcea)

NASA Astrophysics Data System (ADS)

Welton, R. F.; Carmichael, J.; Desai, N. J.; Fuga, R.; Goulding, R. H.; Han, B.; Kang, Y.; Lee, S. W.; Murray, S. N.; Pennisi, T.; Potter, K. G.; Santana, M.; Stockli, M. P.

2010-02-01

The U.S. Spallation Neutron Source (SNS) is an accelerator-based, pulsed neutron-scattering facility, currently in the process of ramping up neutron production. In order to ensure that the SNS will meet its operational commitments as well as provide for future facility upgrades with high reliability, we are developing a rf-driven, H- ion source based on a water-cooled, ceramic aluminum nitride (AlN) plasma chamber. To date, early versions of this source have delivered up to 42 mA to the SNS front end and unanalyzed beam currents up to ˜100 mA (60 Hz, 1 ms) to the ion source test stand. This source was operated on the SNS accelerator from February to April 2009 and produced ˜35 mA (beam current required by the ramp up plan) with availability of ˜97%. During this run several ion source failures identified reliability issues, which must be addressed before the source re-enters production: plasma ignition, antenna lifetime, magnet cooling, and cooling jacket integrity. This report discusses these issues, details proposed engineering solutions, and notes progress to date.

Sputtering Erosion in Ion and Plasma Thrusters

NASA Technical Reports Server (NTRS)

Ray, Pradosh K.

1996-01-01

Low energy sputtering of molybdenum, tantalum and boron nitride with xenon ions are being studied using secondary neutral and secondary ion mass spectrometry (SNMS/SIMS). An ultrahigh vacuum chamber was used to conduct the experiment at a base pressure of 1x10(exp -9) torr. The primary ion beam is generated by an ion gun which is capable of delivering ion currents in the range of 20 to 500 nA. The ion beam can be focused to a spot size of approximately 1 mm in diameter. The mass spectrometer is positioned 10 mm from the target and 90 deg to the primary ion beam direction. SNMS and SIMS spectra were collected at various incident angles and different ion energies. For boron nitride sputtering, the target was flooded with an electron beam to neutralize the charge buildup on the surface. In the SNMS mode, sputtering of Mo and Ta can be detected at an ion energy as low as 100 eV whereas in boron nitride the same was observed up to an energy of 300 eV. However, in the positive-SIMS mode, the sputtering of Mo was observed at 10 eV incident ion energy. The SIMS spectra obtained for boron nitride clearly identifies the two isotopes of boron as well as cluster ions such as B2(sup +) and molecular ions such as BN(sup +). From the angle versus yields measurements, it was found that the maximum SNMS yield shifts towards lower incident angles at low ion energies for all three samples.

Enhanced optoelectronic performances of vertically aligned hexagonal boron nitride nanowalls-nanocrystalline diamond heterostructures

NASA Astrophysics Data System (ADS)

Sankaran, Kamatchi Jothiramalingam; Hoang, Duc Quang; Kunuku, Srinivasu; Korneychuk, Svetlana; Turner, Stuart; Pobedinskas, Paulius; Drijkoningen, Sien; van Bael, Marlies K.; D' Haen, Jan; Verbeeck, Johan; Leou, Keh-Chyang; Lin, I.-Nan; Haenen, Ken

2016-07-01

Field electron emission (FEE) properties of vertically aligned hexagonal boron nitride nanowalls (hBNNWs) grown on Si have been markedly enhanced through the use of nitrogen doped nanocrystalline diamond (nNCD) films as an interlayer. The FEE properties of hBNNWs-nNCD heterostructures show a low turn-on field of 15.2 V/μm, a high FEE current density of 1.48 mA/cm2 and life-time up to a period of 248 min. These values are far superior to those for hBNNWs grown on Si substrates without the nNCD interlayer, which have a turn-on field of 46.6 V/μm with 0.21 mA/cm2 FEE current density and life-time of 27 min. Cross-sectional TEM investigation reveals that the utilization of the diamond interlayer circumvented the formation of amorphous boron nitride prior to the growth of hexagonal boron nitride. Moreover, incorporation of carbon in hBNNWs improves the conductivity of hBNNWs. Such a unique combination of materials results in efficient electron transport crossing nNCD-to-hBNNWs interface and inside the hBNNWs that results in enhanced field emission of electrons. The prospective application of these materials is manifested by plasma illumination measurements with lower threshold voltage (370 V) and longer life-time, authorizing the role of hBNNWs-nNCD heterostructures in the enhancement of electron emission.

Design of Metastable Tin Titanium Nitride Semiconductor Alloys

DOE PAGES

Bikowski, Andre; Siol, Sebastian; Gu, Jing; ...

2017-07-07

Here, we report on design of optoelectronic properties in previously unreported metastable tin titanium nitride alloys with spinel crystal structure. Theoretical calculations predict that Ti alloying in metastable Sn 3N 4 compound should improve hole effective mass by up to 1 order of magnitude, while other optical bandgaps remains in the 1–2 eV range up to x ~ 0.35 Ti composition. Experimental synthesis of these metastable alloys is predicted to be challenging due to high required nitrogen chemical potential (Δμ N ≥ +1.0 eV) but proven to be possible using combinatorial cosputtering from metal targets in the presence of nitrogenmore » plasma. Characterization experiments confirm that thin films of such (Sn 1–xTi x) 3N 4 alloys can be synthesized up to x = 0.45 composition, with suitable optical band gaps (1.5–2.0 eV), moderate electron densities (10 17 to 10 18 cm –3), and improved photogenerated hole transport (by 5×). Overall, this study shows that it is possible to design the metastable nitride materials with properties suitable for potential use in solar energy conversion applications.« less

Drude analysis of transition metal nitride films for solar control and low-E multilayers

NASA Astrophysics Data System (ADS)

Veszelei, Monica; Ribbing, Carl-Gustaf; Roos, Arne

1994-09-01

The Drude-like behavior of the group IVB metal nitrides: TiN, ZrN and HfN furnishes the physical basis for the use of these hard, inert materials as replacement for noble metals in optically selective multilayers. A low value of the refractive index, n, in the visible region and rapidly increasing extinction coefficient, k, when the wavelength increases into the infrared, is characteristic for these nitrides, although to a lesser extent than for the noble metals. A screened Drude model can be fitted to the experimental dielectric function over the near infrared and at least part of the visible spectrum to determine the parameters: plasma resonance energy hvp and relaxation time (tau) . Systematic studies of TiN and ZrN films show that n increases with decreasing film thickness below 60 nm when the film transmits. This increase can be modelled with a increasing Drude parameter (tau) and has previously been explained as an extrinsic effect from defects etc. It is argued that most of this change can be understood as an effect of diffuse scattering against the back surface of the film and is therefore not cured by improvements in deposition technology.

Comparison of the surface charge behavior of commercial silicon nitride and silicon carbide powders

NASA Technical Reports Server (NTRS)

Whitman, Pamela K.; Feke, Donald L.

1988-01-01

The adsorption and desorption of protons from aqueous solution onto the surfaces of a variety of commercial silicon carbide and silicon nitride powders has been examined using a surface titration methodology. This method provides information on some colloidal characteristics, such as the point of zero charge (pzc) and the variation of proton adsorption with dispersion pH, useful for the prediction of optimal ceramic-processing conditions. Qualitatively, the magnitude of the proton adsorption from solution reveals small differences among all of the materials studied. However, the results show that the pzc for the various silicon nitride powders is affected by the powder synthesis route. Complementary investigations have shown that milling can also act to shift the pzc exhibited by silicon nitride powder. Also, studies of the role of the electrolyte in the development of surface charge have indicated no evidence of specific adsorption of ammonium ion on either silicon nitride or silicon carbide powders.

Electrode structure and method for making the same

DOEpatents

Affinito, John D.; Lowe, Gregory K.

2015-05-26

Electrode structures, and more specifically, electrode structures for use in electrochemical cells, are provided. The electrode structures described herein may include one or more protective layers. In one set of embodiments, a protective layer may be formed by exposing a lithium metal surface to a plasma comprising ions of a gas to form a ceramic layer on top of the lithium metal. The ceramic layer may be highly conductive to lithium ions and may protect the underlying lithium metal surface from reaction with components in the electrolyte. In some cases, the ions may be nitrogen ions and a lithium nitride layer may be formed on the lithium metal surface. In other embodiments, the protective layer may be formed by converting lithium to lithium nitride at high pressures. Other methods for forming protective layers are also provided.

Patterning monolayer graphene with zigzag edges on hexagonal boron nitride by anisotropic etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Guole; Wu, Shuang; Zhang, Tingting

2016-08-01

Graphene nanostructures are potential building blocks for nanoelectronic and spintronic devices. However, the production of monolayer graphene nanostructures with well-defined zigzag edges remains a challenge. In this paper, we report the patterning of monolayer graphene nanostructures with zigzag edges on hexagonal boron nitride (h-BN) substrates by an anisotropic etching technique. We found that hydrogen plasma etching of monolayer graphene on h-BN is highly anisotropic due to the inert and ultra-flat nature of the h-BN surface, resulting in zigzag edge formation. The as-fabricated zigzag-edged monolayer graphene nanoribbons (Z-GNRs) with widths below 30 nm show high carrier mobility and width-dependent energy gaps atmore » liquid helium temperature. These high quality Z-GNRs are thus ideal structures for exploring their valleytronic or spintronic properties.« less

Enhanced c-axis orientation of aluminum nitride thin films by plasma-based pre-conditioning of sapphire substrates for SAW applications

NASA Astrophysics Data System (ADS)

Gillinger, M.; Shaposhnikov, K.; Knobloch, T.; Stöger-Pollach, M.; Artner, W.; Hradil, K.; Schneider, M.; Kaltenbacher, M.; Schmid, U.

2018-03-01

Aluminum nitride (AlN) on sapphire has been investigated with two different pretreatments prior to sputter deposition of the AlN layer to improve the orientation and homogeneity of the thin film. An inverse sputter etching of the substrate in argon atmosphere results in an improvement of the uniformity of the alignment of the AlN grains and hence, in enhanced electro-mechanical AlN film properties. This effect is demonstrated in the raw measurements of SAW test devices. Additionally, the impulse response of several devices shows that a poor AlN thin film layer quality leads to a higher signal damping during the transduction of energy in the inter-digital transducers. As a result, the triple-transit signal cannot be detected at the receiver.

Microstructure and wear resistance of one-step in-situ synthesized TiN/Al composite coatings on Ti6Al4V alloy by a laser nitriding process

NASA Astrophysics Data System (ADS)

Fu, Yao; Zhang, Xian-Cheng; Sui, Jian-Feng; Tu, Shan-Tung; Xuan, Fu-Zhen; Wang, Zheng-Dong

2015-04-01

The aim of this paper was to develop a one-step in situ method to synthesize the TiN reinforced Al metallic matrix composite coatings on Ti6Al4V alloy. In this method, the Al powder and nitrogen gas were simultaneously fed into feeding nozzle during a laser nitriding process. The microstructure, microhardness and sliding wear resistance of TiN/Al coatings synthesized at different laser powers in laser nitriding were investigated. Results showed that the crack- and pore-free coatings can be made through the proposed method. However, the morphologies and distribution of TiN dendrites and wear resistance of coatings were strongly dependent on laser power used in nitriding. With increasing the laser power, the amount and density of massive TiN dendritic structure in the coating decreased and the elongated and narrow dendrites increased, leading to the increment of wear resistance of coating. When the laser power is high, the convectional flow pattern of the melt pool can be seen near the bottom of pool.

Synthesis of Silicon Nitride and Silicon Carbide Nanocomposites through High Energy Milling of Waste Silica Fume for Structural Applications

NASA Astrophysics Data System (ADS)

Suri, Jyothi

Nanocomposites have been widely used in a multitude of applications in electronics and structural components because of their improved mechanical, electrical, and magnetic properties. Silicon nitride/Silicon carbide (Si 3N4/SiC) nanocomposites have been studied intensively for low and high temperature structural applications, such as turbine and automobile engine components, ball bearings, turbochargers, as well as energy applications due to their superior wear resistance, high temperature strength, high oxidation resistance and good creep resistance. Silica fume is the waste material produced during the manufacture of silicon and ferro-silicon alloys, and contains 94 to 97 wt.% SiO2. In the present dissertation, the feasibility of using waste silica fume as the raw material was investigated to synthesize (I) advanced nanocomposites of Si3N4/SiC, and (2) porous silicon carbide (SiC) for membrane applications. The processing approach used to convert the waste material to advanced ceramic materials was based on a novel process called, integrated mechanical and thermal activation process (IMTA) process. In the first part of the dissertation, the effect of parameters such as carbothermic nitridation and reduction temperature and the graphite concentration in the starting silica fume plus graphite mixture, were explored to synthesize nanocomposite powders with tailored amounts of Si3N4 and SiC phases. An effective way to synthesize carbon-free Si3N 4/SiC composite powders was studied to provide a clear pathway and fundamental understanding of the reaction mechanisms. Si3N4/SiC nanocomposite powders were then sintered using two different approaches, based on liquid phase sintering and spark plasma sintering processes, with Al 2O3 and Y2O3 as the sintering aids. The nanocomposites were investigated for their densification behavior, microstructure, and mechanical properties. Si3N4/SiC nanocomposites thus obtained were found to possess superior mechanical properties at much lower costs. The second part of the work has comprised of the successful fabrication of bilayered SiC membranes with a graded porosity, consisting of porous nano-SiC layer on the surface of a porous coarse-grained SiC support layer. The effect of different particle sizes of SiC in the support layers was systematically studied. Also, the effects of sintering temperature were investigated to control the pore size, particle size and overall density of the bi-layered SiC membrane.

Bottom-Up Syntheses and Characterization of One Dimensional Nanomaterials

NASA Astrophysics Data System (ADS)

Yeh, Yao-Wen

Nanomaterials, materials having at least one dimension below 100 nm, have been creating exciting opportunities for fundamental quantum confinement studies and applications in electronic devices and energy technologies. One obvious and important aspect of nanomaterials is their production. Although nanostructures can be obtained by top-down reductive e-beam lithography and focused ion beam processes, further development of these processes is needed before these techniques can become practical routes to large scale production. On the other hand, bottom-up syntheses, with advantages in material diversity, throughput, and the potential for large volume production, may provide an alternative strategy for creating nanostructures. In this work, we explore syntheses of one dimensional nanostructures based on hydrothermal and arc discharge methods. The first project presented in this thesis involves syntheses of technologically important nanomaterials and their potential application in energy harvesting. In particular, it was demonstrated that single crystal ferroelectric lead magnesium niobate lead titanate (PMN-PT) nanowires can be synthesized by a hydrothermal route. The chemical composition of the synthesized nanowires is near the rhombohedral-monoclinic boundary of PMN-PT, which leads to a high piezoelectric coefficient of 381 pm/V. Finally, the potential use of PMN-PT nanowires in energy harvesting applications was also demonstrated. The second part of this thesis involves the synthesis of carbon and boron nitride nanotubes by dc arc discharges. In particular, we investigated how local plasma related properties affected the synthesis of carbon nanostructures. Finally, we investigated the anodic nature of the arc and how a dc arc discharge can be applied to synthesize boron nitride nanotubes.

Functionalizing carbon nitride with heavy atom-free spin converters for enhanced 1 O 2 generation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Wenting; Han, Congcong; Zhang, Qinhua

advanced photosensitizers for singlet oxygen (1O2) generation. However, the intersystem crossing (ISC) process is quite insufficient in carbon nitride, limiting the 1O2 generation. Here, we report a facile and general strategy to confined benzophenone as a heavy atom-free spin converter dopant in carbon nitride via the facile copolymerization. With proper energy level matching between the heavy atom-free spin converter and various ligands based on carbon nitride precursors, the proper combination can decrease the singlet-triplet energy gap (DEST) and hence generate 1O2 effectively. Due to its significant and selectivity for 1O2 generation, the as-prepared carbon nitride-based photosensitizer shows a high selectivemore » photooxidation activity for 1,5-dihydroxy-naphthalene (1,5-DHN). The product yield reached 71.8% after irradiation for 60 min, which was higher than that of cyclometalated PtII complexes (53.6%) in homogeneous photooxidation. This study can broaden the application of carbon nitride in the field of selective heterogeneous photooxidation due to simple operation, low cost, and high efficiency, making it a strong candidate for future industrialization.« less

Carbon nanotube, graphene and boron nitride nanotube reinforced bioactive ceramics for bone repair.

PubMed

Gao, Chengde; Feng, Pei; Peng, Shuping; Shuai, Cijun

2017-10-01

The high brittleness and low strength of bioactive ceramics have severely restricted their application in bone repair despite the fact that they have been regarded as one of the most promising biomaterials. In the last few years, low-dimensional nanomaterials (LDNs), including carbon nanotubes, graphene and boron nitride nanotubes, have gained increasing attention owing to their favorable biocompatibility, large surface specific area and super mechanical properties. These qualities make LDNs potential nanofillers in reinforcing bioactive ceramics. In this review, the types, characteristics and applications of the commonly used LDNs in ceramic composites are summarized. In addition, the fabrication methods for LDNs/ceramic composites, such as hot pressing, spark plasma sintering and selective laser sintering, are systematically reviewed and compared. Emphases are placed on how to obtain the uniform dispersion of LDNs in a ceramic matrix and maintain the structural stability of LDNs during the high-temperature fabrication process of ceramics. The reinforcing mechanisms of LDNs in ceramic composites are then discussed in-depth. The in vitro and in vivo studies of LDNs/ceramic in bone repair are also summarized and discussed. Finally, new developments and potential applications of LDNs/ceramic composites are further discussed with reference to experimental and theoretical studies. Despite bioactive ceramics having been regarded as promising biomaterials, their high brittleness and low strength severely restrict their application in bone scaffolds. In recent years, low-dimensional nanomaterials (LDNs), including carbon nanotubes, graphene and boron nitride nanotubes, have shown great potential in reinforcing bioactive ceramics owing to their unique structures and properties. However, so far it has been difficult to maintain the structural stability of LDNs during fabrication of LDNs/ceramic composites, due to the lengthy, high-temperature process involved. This review presents a comprehensive overview of the developments and applications of LDNs in bioactive ceramics. The newly-developed fabrication methods for LDNs/ceramic composites, the reinforcing mechanisms and the in vitro and in vivo performance of LDNs are also summarized and discussed in detail. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Synthesis of gallium nitride nanostructures by nitridation of electrochemically deposited gallium oxide on silicon substrate.

PubMed

Ghazali, Norizzawati Mohd; Yasui, Kanji; Hashim, Abdul Manaf

2014-01-01

Gallium nitride (GaN) nanostructures were successfully synthesized by the nitridation of the electrochemically deposited gallium oxide (Ga2O3) through the utilization of a so-called ammoniating process. Ga2O3 nanostructures were firstly deposited on Si substrate by a simple two-terminal electrochemical technique at a constant current density of 0.15 A/cm(2) using a mixture of Ga2O3, HCl, NH4OH and H2O for 2 h. Then, the deposited Ga2O3 sample was ammoniated in a horizontal quartz tube single zone furnace at various ammoniating times and temperatures. The complete nitridation of Ga2O3 nanostructures at temperatures of 850°C and below was not observed even the ammoniating time was kept up to 45 min. After the ammoniating process at temperature of 900°C for 15 min, several prominent diffraction peaks correspond to hexagonal GaN (h-GaN) planes were detected, while no diffraction peak of Ga2O3 structure was detected, suggesting a complete transformation of Ga2O3 to GaN. Thus, temperature seems to be a key parameter in a nitridation process where the deoxidization rate of Ga2O3 to generate gaseous Ga2O increase with temperature. The growth mechanism for the transformation of Ga2O3 to GaN was proposed and discussed. It was found that a complete transformation can not be realized without a complete deoxidization of Ga2O3. A significant change of morphological structures takes place after a complete transformation of Ga2O3 to GaN where the original nanorod structures of Ga2O3 diminish, and a new nanowire-like GaN structures appear. These results show that the presented method seems to be promising in producing high-quality h-GaN nanostructures on Si.

Synthesis of gallium nitride nanostructures by nitridation of electrochemically deposited gallium oxide on silicon substrate

PubMed Central

2014-01-01

Gallium nitride (GaN) nanostructures were successfully synthesized by the nitridation of the electrochemically deposited gallium oxide (Ga2O3) through the utilization of a so-called ammoniating process. Ga2O3 nanostructures were firstly deposited on Si substrate by a simple two-terminal electrochemical technique at a constant current density of 0.15 A/cm2 using a mixture of Ga2O3, HCl, NH4OH and H2O for 2 h. Then, the deposited Ga2O3 sample was ammoniated in a horizontal quartz tube single zone furnace at various ammoniating times and temperatures. The complete nitridation of Ga2O3 nanostructures at temperatures of 850°C and below was not observed even the ammoniating time was kept up to 45 min. After the ammoniating process at temperature of 900°C for 15 min, several prominent diffraction peaks correspond to hexagonal GaN (h-GaN) planes were detected, while no diffraction peak of Ga2O3 structure was detected, suggesting a complete transformation of Ga2O3 to GaN. Thus, temperature seems to be a key parameter in a nitridation process where the deoxidization rate of Ga2O3 to generate gaseous Ga2O increase with temperature. The growth mechanism for the transformation of Ga2O3 to GaN was proposed and discussed. It was found that a complete transformation can not be realized without a complete deoxidization of Ga2O3. A significant change of morphological structures takes place after a complete transformation of Ga2O3 to GaN where the original nanorod structures of Ga2O3 diminish, and a new nanowire-like GaN structures appear. These results show that the presented method seems to be promising in producing high-quality h-GaN nanostructures on Si. PMID:25593562

Insulators obtained by electron cyclotron resonance plasmas on Si or GaAs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diniz, J.A.; Doi, I.; Swart, J.W

2003-03-15

Silicon oxynitride (SiO{sub x}N{sub y}) and nitride (SiN{sub x}) insulators have been deposited or grown (with or without silane in the gas mixture, respectively) by electron cyclotron resonance (ECR) plasmas on Si and/or GaAs substrates at room temperature (20 deg. C) and low pressures (up to 10 mTorr). Chemical bonding characteristics of the SiO{sub x}N{sub y} and SiN{sub x} films were evaluated using Fourier transform infrared spectrometry (FTIR). The profile measurements determined the film thickness, the deposition (or oxidation) rate and the etch rates in buffered HF (BHF). The refractive indexes and the thicknesses were determined by ellipsometry. The effectivemore » interface charge densities were determined by capacitance-voltage (C-V) measurements. With these processes and analyses, different films were obtained and optimized. Suitable gate insulators for metal-insulator-semiconductor (MIS) devices with low interface charge densities were developed: (a) SiN{sub x} films deposited by ECR-chemical vapor deposition (ECR-PECVD) on GaAs substrates; (b) SiO{sub x}N{sub y} insulators obtained by low-energy molecular nitrogen ion ({sup 28}N{sub 2}{sup +}) implantation (energy of 5 keV and dose of 1x10{sup 15}/cm{sup 2}) in Si substrates prior to high-density O{sub 2} ECR plasma oxidation; and (c) SiO{sub x}N{sub y} insulators grown (without silane in the gas mixture) by O{sub 2}/N{sub 2}/Ar ECR plasma 'oxynitridation'. Furthermore, some SiN{sub x} films also present very good masking characteristics for local oxidation of silicon process.« less

Theoretical study of the ammonia nitridation rate on an Fe (100) surface: A combined density functional theory and kinetic Monte Carlo study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yeo, Sang Chul; Lee, Hyuck Mo, E-mail: hmlee@kaist.ac.kr; Lo, Yu Chieh

2014-10-07

Ammonia (NH{sub 3}) nitridation on an Fe surface was studied by combining density functional theory (DFT) and kinetic Monte Carlo (kMC) calculations. A DFT calculation was performed to obtain the energy barriers (E{sub b}) of the relevant elementary processes. The full mechanism of the exact reaction path was divided into five steps (adsorption, dissociation, surface migration, penetration, and diffusion) on an Fe (100) surface pre-covered with nitrogen. The energy barrier (E{sub b}) depended on the N surface coverage. The DFT results were subsequently employed as a database for the kMC simulations. We then evaluated the NH{sub 3} nitridation rate onmore » the N pre-covered Fe surface. To determine the conditions necessary for a rapid NH{sub 3} nitridation rate, the eight reaction events were considered in the kMC simulations: adsorption, desorption, dissociation, reverse dissociation, surface migration, penetration, reverse penetration, and diffusion. This study provides a real-time-scale simulation of NH{sub 3} nitridation influenced by nitrogen surface coverage that allowed us to theoretically determine a nitrogen coverage (0.56 ML) suitable for rapid NH{sub 3} nitridation. In this way, we were able to reveal the coverage dependence of the nitridation reaction using the combined DFT and kMC simulations.« less

Efficient Boron-Carbon-Nitrogen Nanotube Formation Via Combined Laser-Gas Flow Levitation

NASA Technical Reports Server (NTRS)

Whitney, R. Roy (Inventor); Smith, Michael W. (Inventor); Jordan, Kevin (Inventor)

2015-01-01

A process for producing boron nitride nanotubes and/or boron-carbon-nitrogen nanotubes of the general formula BxCyNz. The process utilizes a combination of laser light and nitrogen gas flow to support a boron ball target during heating of the boron ball target and production of a boron vapor plume which reacts with nitrogen or nitrogen and carbon to produce boron nitride nanotubes and/or boron-carbon-nitrogen nanotubes of the general formula BxCyNz.

Processing and testing of high toughness silicon nitride ceramics

NASA Technical Reports Server (NTRS)

Tikare, Veena; Sanders, William A.; Choi, Sung R.

1993-01-01

High toughness silicon nitride ceramics were processed with the addition of small quantities of beta-Si3N4 whiskers in a commercially available alpha-Si3N4 powder. These whiskers grew preferentially during sintering resulting in large, elongated beta-grains, which acted to toughen the matrix by crack deflection and grain pullout. The fracture toughness of these samples seeded with beta-Si3N4 whiskers ranged from 8.7 to 9.5 MPa m(exp 0.5) depending on the sintering additives.

Method for exfoliation of hexagonal boron nitride

NASA Technical Reports Server (NTRS)

Lin, Yi (Inventor); Connell, John W. (Inventor)

2012-01-01

A new method is disclosed for the exfoliation of hexagonal boron nitride into mono- and few-layered nanosheets (or nanoplatelets, nanomesh, nanoribbons). The method does not necessarily require high temperature or vacuum, but uses commercially available h-BN powders (or those derived from these materials, bulk crystals) and only requires wet chemical processing. The method is facile, cost efficient, and scalable. The resultant exfoliated h-BN is dispersible in an organic solvent or water thus amenable for solution processing for unique microelectronic or composite applications.

Growth kinetics and characterizations of gallium nitride thin films by remote PECVD

NASA Technical Reports Server (NTRS)

Choi, S. W.; Bachmann, K. J.; Lucovsky, G.

1993-01-01

Thin films of GaN have been deposited at relatively low growth temperatures by remote plasma-enhanced chemical-vapor deposition (RPECVD), using a plasma excited NH3, and trimethylgallium (TMG), injected downstream from the plasma. The activation energy for GaN growth has been tentatively assigned to the dissociation of NH groups as the primary N-atom precursors in the surface reaction with adsorbed TMG, or TMG fragments. At high He flow rates, an abrupt increase in the growth rate is observed and corresponds to a change in the reaction mechanism attributed to the formation of atomic N. XRD reveals an increased tendency to ordered growth in the (0001) direction with increasing growth temperature, He flow rate, and RF plasma power. IR spectra show the fundamental lattice mode of GaN at 530 cm without evidence for vibrational modes of hydrocarbon groups.

An optical probe for local measurements of fast plasma ion dynamics

NASA Astrophysics Data System (ADS)

Fiksel, G.; Den Hartog, D. J.; Fontana, P. W.

1998-05-01

A novel insertable probe for local measurements of equilibrium and fluctuating plasma ion flow velocity and temperature via Doppler spectroscopy is described. Optical radiation is collected by two fused silica fiber optic bundles with perpendicular viewlines. Spatial resolution of about 5 cm is achieved by terminating each view with an optical dump. The collected light is transported by the fiber bundles to a high-resolution spectrometer. Two components of the velocity are measured simultaneously—the radial along the insertion of the probe and a perpendicular component (which can be varied by simply rotating the probe by 90°). The accuracy of the velocity measurements is better than 1 km/s. The probe is armored by a boron nitride enclosure and is inserted into a high temperature plasma to obtain radial profiles of the equilibrium and fluctuating plasma velocity. Initial measurements have been done in Madison Symmetric Torus reversed field pinch.

Modeling the mechanical behavior of ceramic and heterophase structures manufactured using selective laser sintering and spark plasma sintering

NASA Astrophysics Data System (ADS)

Skripnyak, Vladimir A.; Skripnyak, Evgeniya G.; Skripnyak, Vladimir V.; Vaganova, Irina K.

A model for predicting mechanical properties of ultra-high temperature ceramics and composites manufactured by selective laser sintering (SLS) and spark plasma sintering (SPS) under shock loading is presented. The model takes into account the porous structure, the specific volume and average sizes of phases, and the temperature of sintering. Residual stresses in ceramic composites reinforced with particles of refractory borides, carbides and nitrides after SLS or SPS were calculated. It is shown that the spall strength of diboride-zirconium matrix composites can be increased by the decreasing of porosity and the introduction of inclusions of specially selected refractory strengthening phases.

Energy efficiency in nanoscale synthesis using nanosecond plasmas

PubMed Central

Pai, David Z.; (Ken) Ostrikov, Kostya; Kumar, Shailesh; Lacoste, Deanna A.; Levchenko, Igor; Laux, Christophe O.

2013-01-01

We report a nanoscale synthesis technique using nanosecond-duration plasma discharges. Voltage pulses 12.5 kV in amplitude and 40 ns in duration were applied repetitively at 30 kHz across molybdenum electrodes in open ambient air, generating a nanosecond spark discharge that synthesized well-defined MoO3 nanoscale architectures (i.e. flakes, dots, walls, porous networks) upon polyamide and copper substrates. No nitrides were formed. The energy cost was as low as 75 eV per atom incorporated into a nanostructure, suggesting a dramatic reduction compared to other techniques using atmospheric pressure plasmas. These findings show that highly efficient synthesis at atmospheric pressure without catalysts or external substrate heating can be achieved in a simple fashion using nanosecond discharges. PMID:23386976

Characterization of Ti and Co based biomaterials processed via laser based additive manufacturing

NASA Astrophysics Data System (ADS)

Sahasrabudhe, Himanshu

Titanium and Cobalt based metallic materials are currently the most ideal materials for load-bearing metallic bio medical applications. However, the long term tribological degradation of these materials still remains a problem that needs a solution. To improve the tribological performance of these two metallic systems, three different research approaches were adapted, stemming out four different research projects. First, the simplicity of laser gas nitriding was utilized with a modern LENS(TM) technology to form an in situ nitride rich later in titanium substrate material. This nitride rich composite coating improved the hardness by as much as fifteen times and reduced the wear rate by more than a magnitude. The leaching of metallic ions during wear was also reduced by four times. In the second research project, a mixture of titanium and silicon were processed on a titanium substrate in a nitrogen rich environment. The results of this reactive, in situ additive manufacturing process were Ti-Si-Nitride coatings that were harder than the titanium substrate by more than twenty times. These coatings also reduced the wear rate by more than two magnitudes. In the third research approach, composites of CoCrMo alloy and Calcium phosphate (CaP) bio ceramic were processed using LENS(TM) based additive manufacturing. These composites were effective in reducing the wear in the CoCrMo alloy by more than three times as well as reduce the leaching of cobalt and chromium ions during wear. The novel composite materials were found to develop a tribofilm during wear. In the final project, a combination of hard nitride coating and addition of CaP bioceramic was investigated by processing a mixture of Ti6Al4V alloy and CaP in a nitrogen rich environment using the LENS(TM) technology. The resultant Ti64-CaP-Nitride coatings significantly reduced the wear damage on the substrate. There was also a drastic reduction in the metal ions leached during wear. The results indicate that the three tested approaches for reducing the wear damage in Ti and Co based were successful. These approaches and the associated research investigations could pave the way for future work in alleviating wear and corrosion related damage, especially via the additive manufacturing route.

Chemical reaction of hexagonal boron nitride and graphite nanoclusters in mechanical milling systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muramatsu, Y.; Grush, M.; Callcott, T.A.

1997-04-01

Synthesis of boron-carbon-nitride (BCN) hybrid alloys has been attempted extensively by many researchers because the BCN alloys are considered an extremely hard material called {open_quotes}super diamond,{close_quotes} and the industrial application for wear-resistant materials is promising. A mechanical alloying (MA) method of hexagonal boron nitride (h-BN) with graphite has recently been studied to explore the industrial synthesis of the BCN alloys. To develop the MA method for the BCN alloy synthesis, it is necessary to confirm the chemical reaction processes in the mechanical milling systems and to identify the reaction products. Therefore, the authors have attempted to confirm the chemical reactionmore » process of the h-BN and graphite in mechanical milling systems using x-ray absorption near edge structure (XANES) methods.« less

Extraction of Boron Nitride Nanotubes and Fabrication of Macroscopic Articles Using Chlorosulfonic Acid.

PubMed

Adnan, Mohammed; Marincel, Daniel M; Kleinerman, Olga; Chu, Sang-Hyon; Park, Cheol; Hocker, Samuel J A; Fay, Catharine; Arepalli, Sivaram; Talmon, Yeshayahu; Pasquali, Matteo

2018-03-14

Due to recent advances in high-throughput synthesis, research on boron nitride nanotubes (BNNTs) is moving toward applications. One future goal is the assembly of macroscopic articles of high-aspect-ratio, pristine BNNTs. However, these articles are presently unattainable because of insufficient purification and fabrication methods. We introduce a solution process for extracting BNNTs from synthesis impurities without sonication or the use of surfactants and proceed to convert the extracted BNNTs into thin films. The solution process can also be used to convert as-synthesized material-which contains significant amounts of hexagonal boron nitride ( h-BN)-into mats and aerogels with controllable structure and dimension. The solution extraction method, combined with further advances in synthesis and purification, contributes to the development of all-BNNT macroscopic articles, such as fibers and 3-D structures.

Nitriding kinetics of Si-SiC powder mixtures as simulations of reaction bonded Si3N4-SiC composites

NASA Technical Reports Server (NTRS)

Lightfoot, A.; Sheldon, B. W.; Flint, J. H.; Haggerty, J. S.

1989-01-01

The nitriding kinetics of Si and Si plus SiC powder mixtures were studied to simulate the fabrication of RBSN-SiC ceramic matrix composites. Very clean, assynthesized, and solvent-exposed powders were studied; C-rich and Si-rich SiC 0.04-0.05 micron diameter powders were mixed in varying concentrations with SiH4-derived 0.2-0.3 micron diameter Si powder. Complete nitridation is achieved with C-rich SiC powders in 140 min at 1250 C, and in the centers of Si-rich SiC powders in 15 min. The effects on the incubation periods, fast reaction periods, and slow reaction periods that characterize these nitriding processes were studied to explain unusual reverse reaction gradients and other effects of contamination.

Process for preparing titanium nitride powder

DOEpatents

Bamberger, C.E.

1988-06-17

A process for making titanium nitride powder by reaction of titanium phosphates with sodium cyanide. The process of this invention may comprise mixing one or more phosphates of Ti with a cyanide salt in the absence of oxygen and heating to a temperature sufficient to cause reaction to occur. In the preferred embodiment the ratio of cyanide salt to Ti should be at least 2 which results in the major Ti-containing product being TiN rather than sodium titanium phosphate byproducts. The process is an improvement over prior processes since the byproducts are water soluble salts of sodium which can easily be removed from the preferred TiN product by washing. 2 tabs.

Shear strength of a three-dimensional capillary-porous titanium coating for biomedical applications

NASA Astrophysics Data System (ADS)

Kalita, V. I.; Komlev, D. I.; Radyuk, A. A.; Ivannikov, A. Yu; Alpatov, A. V.; Komlev, V. S.; Mamonov, V. I.; Sevostyanov, M. A.; Baikin, A. S.

2018-04-01

The effect of pretreatment and plasma preheating of Ti-substrate on shear strength of three-dimensional capillary porous Ti-coating was studied. After sandblasting the shear strength of the plasma sprayed coating was 200 ± 2 MPa, and after additional matting it was 68 ± 4 MPa. The use of plasma preheating of the substrates for 9 seconds decreased difference between values of the shear strength to 249 ± 17 MPa and 229 ± 16 MPa, respectively. After plasma spraying the microhardness of the surface layer of the substrate was 4.34 ± 0.35 GPa, the microhardness of the boundary between the coating and the substrate was 8.08 ± 0.45 GPa, and the microhardness of the coating was 3.48 ± 0.25 GPa. High shear strength of the coating was attributed to the activation of the substrate by means of plasma preheating and hardening of the boundary between the coating and the substrate by oxides and nitrides.

Plasma enhanced chemical vapor deposition of titanium nitride thin films using cyclopentadienyl cycloheptatrienyl titanium

NASA Astrophysics Data System (ADS)

Charatan, R. M.; Gross, M. E.; Eaglesham, D. J.

1994-10-01

The use of a low oxidation state Ti compound, cyclopentadienyl cycloheptatrienyl titanium, (C5H5) Ti(C7H7) (CPCHT), as a potential source for TiN and Ti in plasma enhanced chemical vapor deposition processes has been investigated. This precursor provides us with a new chemical vapor deposition route to TiN films that offer an interesting contrast to films deposited from Ti(IV) precursors. Film depositions were carried out by introducing CPCHT, with H2 carrier gas, into the downstream region of a NH3, N2, H2, or mixed H2/N2 plasma. Low resistivity (100-250 micro-ohm cm) nitrogen-rich TiN films with little carbon or oxygen incorporation and good conformality were deposited with activated N2 or NH3 at deposition temperatures of 300-600 C, inclusive. Mixed H2/N2 plasmas resulted in more stoichiometric TiN films with similar properties. The most striking feature of these films is the absence of columnar grain growth, in contrast to TiN films deposited using TiCl4 or Ti(NR(2))(4). Although the film texture was influenced by the plasma gas, the average grain size of the films deposited using activated N2 and NH3 was similar. The TiN films that we deposited were effective diffusion barriers between aluminum and silicon up to 575 C. Depositions using activated H2 resulted in films with significantly less carbon than CPCHT, but still having a minimum of 2.7:1 C:Ti. The lower oxidation state of the precursor did not facilitate the deposition of a Ti-rich film. No depositions were observed with any of the reactant gases in the absence of plasmas activation.

Gallium Nitride (GaN) High Power Electronics (FY11)

DTIC Science & Technology

2012-01-01

GaN films grown by metal-organic chemical vapor deposition (MOCVD) and ~1010 in films grown by molecular beam epitaxy (MBE) when they are deposited...inductively coupled plasma I-V current-voltage L-HVPE low doped HVPE MBE molecular beam epitaxy MOCVD metal-organic chemical vapor deposition...figure of merit HEMT high electron mobility transistor H-HVPE high doped HVPE HPE high power electronics HVPE hydride vapor phase epitaxy ICP

Direct growth of hexagonal boron nitride/graphene heterostructures on cobalt foil substrates by plasma-assisted molecular beam epitaxy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Zhongguang; Khanaki, Alireza; Tian, Hao

2016-07-25

Graphene/hexagonal boron nitride (G/h-BN) heterostructures have attracted a great deal of attention because of their exceptional properties and wide variety of potential applications in nanoelectronics. However, direct growth of large-area, high-quality, and stacked structures in a controllable and scalable way remains challenging. In this work, we demonstrate the synthesis of h-BN/graphene (h-BN/G) heterostructures on cobalt (Co) foil by sequential deposition of graphene and h-BN layers using plasma-assisted molecular beam epitaxy. It is found that the coverage of h-BN layers can be readily controlled on the epitaxial graphene by growth time. Large-area, uniform-quality, and multi-layer h-BN films on thin graphite layersmore » were achieved. Based on an h-BN (5–6 nm)/G (26–27 nm) heterostructure, capacitor devices with Co(foil)/G/h-BN/Co(contact) configuration were fabricated to evaluate the dielectric properties of h-BN. The measured breakdown electric field showed a high value of ∼2.5–3.2 MV/cm. Both I-V and C-V characteristics indicate that the epitaxial h-BN film has good insulating characteristics.« less

Wetting behaviour of carbon nitride nanostructures grown by plasma enhanced chemical vapour deposition technique

NASA Astrophysics Data System (ADS)

Ahmad Kamal, Shafarina Azlinda; Ritikos, Richard; Abdul Rahman, Saadah

2015-02-01

Tuning the wettability of various coating materials by simply controlling the deposition parameters is essential for various specific applications. In this work, carbon nitride (CNx) films were deposited on silicon (1 1 1) substrates using radio-frequency plasma enhanced chemical vapour deposition employing parallel plate electrode configuration. Effects of varying the electrode distance (DE) on the films' structure and bonding properties were investigated using Field emission scanning electron microscopy, Atomic force microscopy, Fourier transform infrared and X-ray photoemission spectroscopy. The wettability of the films was analyzed using water contact angle measurements. At high DE, the CNx films' surface was smooth and uniform. This changed into fibrous nanostructures when DE was decreased. Surface roughness of the films increased with this morphological transformation. Nitrogen incorporation increased with decrease in DE which manifested the increase in both relative intensities of Cdbnd N to Cdbnd C and Nsbnd H to Osbnd H bonds. sp2-C to sp3-C ratio increased as DE decreased due to greater deformation of sp2 bonded carbon at lower DE. The films' characteristics changed from hydrophilic to super-hydrophobic with the decrease in DE. Roughness ratio, surface porosity and surface energy calculated from contact angle measurements were strongly dependent on the morphology, surface roughness and bonding properties of the films.

Silicon nitride and silicon etching by CH{sub 3}F/O{sub 2} and CH{sub 3}F/CO{sub 2} plasma beams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaler, Sanbir S.; Lou, Qiaowei; Donnelly, Vincent M., E-mail: vmdonnelly@uh.edu

2016-07-15

Silicon nitride (SiN, where Si:N ≠ 1:1) films low pressure-chemical vapor deposited on Si substrates, Si films on Ge on Si substrates, and p-Si samples were exposed to plasma beams emanating from CH{sub 3}F/O{sub 2} or CH{sub 3}F/CO{sub 2} inductively coupled plasmas. Conditions within the plasma beam source were maintained at power of 300 W (1.9 W/cm{sup 3}), pressure of 10 mTorr, and total gas flow rate of 10 sccm. X-ray photoelectron spectroscopy was used to determine the thicknesses of Si/Ge in addition to hydrofluorocarbon polymer films formed at low %O{sub 2} or %CO{sub 2} addition on p-Si and SiN. Polymer film thickness decreasedmore » sharply as a function of increasing %O{sub 2} or %CO{sub 2} addition and dropped to monolayer thickness above the transition point (∼48% O{sub 2} or ∼75% CO{sub 2}) at which the polymer etchants (O and F) number densities in the plasma increased abruptly. The C(1s) spectra for the polymer films deposited on p-Si substrates appeared similar to those on SiN. Spectroscopic ellipsometry was used to measure the thickness of SiN films etched using the CH{sub 3}F/O{sub 2} and CH{sub 3}F/CO{sub 2} plasma beams. SiN etching rates peaked near 50% O{sub 2} addition and 73% CO{sub 2} addition. Faster etching rates were measured in CH{sub 3}F/CO{sub 2} than CH{sub 3}F/O{sub 2} plasmas above 70% O{sub 2} or CO{sub 2} addition. The etching of Si stopped after a loss of ∼3 nm, regardless of beam exposure time and %O{sub 2} or %CO{sub 2} addition, apparently due to plasma assisted oxidation of Si. An additional GeO{sub x}F{sub y} peak was observed at 32.5 eV in the Ge(3d) region, suggesting deep penetration of F into Si, under the conditions investigated.« less

Enhanced laser absorption from radiation pressure in intense laser plasma interactions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dollar, F.; Zulick, C.; Raymond, A.

The reflectivity of a short-pulse laser at intensities of 2 x 10 21Wcm -2 with ultra-high contrast (10 -15) on sub-micrometer silicon nitride foilswas studied experimentally using varying polarizations and target thicknesses. Furthermore, the reflected intensity and beam quality were found to be relatively constant with respect to intensity for bulk targets. For submicron targets, the measured reflectivity drops substantially without a corresponding increase in transmission, indicating increased conversion of fundamental to other wavelengths and particle heating. The experimental results and trends we observed in 3D particle-in-cell simulations emphasize the critical role of ion motion due to radiation pressure onmore » the absorption process. Ion motion during ultra-short pulses enhances the electron heating, which subsequently transfers more energy to the ions.« less

Enhanced laser absorption from radiation pressure in intense laser plasma interactions

DOE PAGES

Dollar, F.; Zulick, C.; Raymond, A.; ...

2017-06-06

The reflectivity of a short-pulse laser at intensities of 2 x 10 21Wcm -2 with ultra-high contrast (10 -15) on sub-micrometer silicon nitride foilswas studied experimentally using varying polarizations and target thicknesses. Furthermore, the reflected intensity and beam quality were found to be relatively constant with respect to intensity for bulk targets. For submicron targets, the measured reflectivity drops substantially without a corresponding increase in transmission, indicating increased conversion of fundamental to other wavelengths and particle heating. The experimental results and trends we observed in 3D particle-in-cell simulations emphasize the critical role of ion motion due to radiation pressure onmore » the absorption process. Ion motion during ultra-short pulses enhances the electron heating, which subsequently transfers more energy to the ions.« less

A novel in situ synthesis of SiBCN-Zr composites prepared by a sol-gel process and spark plasma sintering.

PubMed

Miao, Yang; Yang, Zhihua; Liang, Bin; Li, Quan; Chen, Qingqing; Jia, Dechang; Cheng, Yi-Bing; Zhou, Yu

2016-08-09

In the work reported here, SiBCN amorphous powders were first prepared by a mechanical alloying technique, employing cubic silicon, graphite and hexagonal boron nitride powders as raw materials. Zirconia was then introduced via sol-gel methods. The resulting powder composite was then consolidated via SPS sintering. The SPS sintering sample was evaluated using XRD, SEM and TEM. XRD reveals a chemical transformation wherein amorphous BN(C) and ZrO2 form the primary ZrC and ZrB2 phases after SPS processing along with SiC and BN(C). Thereafter ZrC reacts with BN(C) completely to form ZrB2. The reaction starts at the temperature of 1500 °C and is complete at the temperature of 1900 °C. The fracture toughness of the sintered composites reaches 4.9 ± 0.2 MPa m(1/2) due to the presence of the laminated structure of the BN(C) phase.

Evaluation of resonating Si cantilevers sputter-deposited with AlN piezoelectric thin films for mass sensing applications

NASA Astrophysics Data System (ADS)

Sökmen, Ü.; Stranz, A.; Waag, A.; Ababneh, A.; Seidel, H.; Schmid, U.; Peiner, E.

2010-06-01

We report on a micro-machined resonator for mass sensing applications which is based on a silicon cantilever excited with a sputter-deposited piezoelectric aluminium nitride (AlN) thin film actuator. An inductively coupled plasma (ICP) cryogenic dry etching process was applied for the micro-machining of the silicon substrate. A shift in resonance frequency was observed, which was proportional to a mass deposited in an e-beam evaporation process on top. We had a mass sensing limit of 5.2 ng. The measurements from the cantilevers of the two arrays revealed a quality factor of 155-298 and a mass sensitivity of 120.34 ng Hz-1 for the first array, and a quality factor of 130-137 and a mass sensitivity of 104.38 ng Hz-1 for the second array. Furthermore, we managed to fabricate silicon cantilevers, which can be improved for the detection in the picogram range due to a reduction of the geometrical dimensions.

Boron nitride nanotube reinforced hydroxyapatite composite: mechanical and tribological performance and in-vitro biocompatibility to osteoblasts.

PubMed

Lahiri, Debrupa; Singh, Virendra; Benaduce, Ana Paula; Seal, Sudipta; Kos, Lidia; Agarwal, Arvind

2011-01-01

This study proposes boron nitride nanotube (BNNT) reinforced hydroxyapatite (HA) as a novel composite material for orthopedic implant applications. The spark plasma sintered (SPS) composite structure shows higher density compared to HA. Minimal lattice mismatch between HA and BNNT leads to coherent bonding and strong interface. HA-4 wt% BNNT composite offers excellent mechanical properties-120% increment in elastic modulus, 129% higher hardness and 86% more fracture toughness, as compared to HA. Improvements in the hardness and fracture toughness are related to grain refinement and crack bridging by BNNTs. HA-BNNT composite also shows 75% improvement in the wear resistance. The wear morphology suggests localized plastic deformation supported by the sliding of outer walls of BNNT. Osteoblast proliferation and cell viability show no adverse effect of BNNT addition. HA-BNNT composite is, thus, envisioned as a potential material for stronger orthopedic implants. Copyright © 2010 Elsevier Ltd. All rights reserved.

Structural-dependent thermal conductivity of aluminium nitride produced by reactive direct current magnetron sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Belkerk, B. E.; Soussou, A.; Carette, M.

This Letter reports the thermal conductivity of aluminium nitride (AlN) thin-films deposited by reactive DC magnetron sputtering on single-crystal silicon substrates (100) with varying plasma and magnetic conditions achieving different crystalline qualities. The thermal conductivity of the films was measured at room temperature with the transient hot-strip technique for film thicknesses ranging from 100 nm to 4000 nm. The thermal conductivity was found to increase with the thickness depending on the synthesis conditions and film microstructure. The conductivity in the bulk region of the films, so-called intrinsic conductivity, and the boundary resistance were in the range [120-210] W m{sup -1}more » K{sup -1} and [2-30 Multiplication-Sign 10{sup -9}] K m{sup 2} W{sup -1}, respectively, in good agreement with microstructures analysed by x-ray diffraction, high-resolution-scanning-electron-microscopy, and transmission-electron-microscopy.« less

Effect of nitrogen plasma afterglow on the surface charge effect resulted during XPS surface analysis of amorphous carbon nitride thin films

NASA Astrophysics Data System (ADS)

Kayed, Kamal

2018-06-01

The aim of this paper is to investigate the relationship between the micro structure and the surface charge effect resulted during XPS surface analysis of amorphous carbon nitride thin films prepared by laser ablation method. The study results show that the charge effect coefficient (E) is not just a correction factor. We found that the changes in this coefficient value due to incorporation of nitrogen atoms into the carbon network are related to the spatial configurations of the sp2 bonded carbon atoms, order degree and sp2 clusters size. In addition, results show that the curve E vs. C(sp3)-N is a characteristic curve of the micro structure. This means that using this curve makes it easy to sorting the samples according to the micro structure (hexagonal rings or chains).

Method for making circular tubular channels with two silicon wafers

DOEpatents

Yu, Conrad M.; Hui, Wing C.

1996-01-01

A two-wafer microcapillary structure is fabricated by depositing boron nitride (BN) or silicon nitride (Si.sub.3 N.sub.4) on two separate silicon wafers (e.g., crystal-plane silicon with [100] or [110] crystal orientation). Photolithography is used with a photoresist to create exposed areas in the deposition for plasma etching. A slit entry through to the silicon is created along the path desired for the ultimate microcapillary. Acetone is used to remove the photoresist. An isotropic etch, e.g., such as HF/HNO.sub.3 /CH.sub.3 COOH, then erodes away the silicon through the trench opening in the deposition layer. A channel with a half-circular cross section is then formed in the silicon along the line of the trench in the deposition layer. Wet etching is then used to remove the deposition layer. The two silicon wafers are aligned and then bonded together face-to-face to complete the microcapillary.

Effects of Fiber Coatings on Tensile Properties of Hi-Nicalon SiC/RBSN Tow Composites

NASA Technical Reports Server (NTRS)

Bhatt, Ramakrishna T.; Hull, David R.

1997-01-01

Uncoated Hi-Nicalon silicon carbide (SiC) fiber tows and those coated with a single surface layer of pyrolytic boron nitride (PBN), double layers of PBN/Si-rich PBN, and boron nitride (BN)/SiC coatings deposited by chemical vapor deposition (CVD) method were infiltrated with silicon slurry and then exposed to N2, for 4 hr at 1200 and 1400 C. Room temperature ultimate tensile fracture loads and microstructural characterization of uncoated and CVD coated Hi-Nicalon SiC fiber reinforced reaction-bonded silicon nitride (RBSN) tow composites were measured to select suitable interface coating(s) stable under RBSN processing conditions. Results indicate that room temperature ultimate fracture loads of the uncoated Hi-Nicalon SiC/RBSN tow composites nitrided at both temperatures were significantly lower than those of the uncoated Hi-Nicalon tows without slurry infiltration. In contrast, all CVD coated Hi-Nicalon SiC/RBSN tow composites retained a greater fraction of the dry tow fracture load after nitridation at 1200 C, but degraded significantly after nitridation at 1400 C. Reaction between metal impurities (Fe and Ni) present in the attrition milled silicon powder and uncoated regions of SiC fibers appears to be the probable cause for fiber degradation.

Advanced ceramic material for high temperature turbine tip seals

NASA Technical Reports Server (NTRS)

Solomon, N. G.; Vogan, J. W.

1978-01-01

Ceramic material systems are being considered for potential use as turbine blade tip gas path seals at temperatures up to 1370 1/4 C. Silicon carbide and silicon nitride structures were selected for study since an initial analysis of the problem gave these materials the greatest potential for development into a successful materials system. Segments of silicon nitride and silicon carbide materials over a range of densities, processed by various methods, a honeycomb structure of silicon nitride and ceramic blade tip inserts fabricated from both materials by hot pressing were tested singly and in combination. The evaluations included wear under simulated engine blade tip rub conditions, thermal stability, impact resistance, machinability, hot gas erosion and feasibility of fabrication into engine components. The silicon nitride honeycomb and low-density silicon carbide using a selected grain size distribution gave the most promising results as rub-tolerant shroud liners. Ceramic blade tip inserts made from hot-pressed silicon nitride gave excellent test results. Their behavior closely simulated metal tips. Wear was similar to that of metals but reduced by a factor of six.

A kinetic model for the thermal nitridation of SiO2/Si

NASA Technical Reports Server (NTRS)

Vasquez, R. P.; Madhukar, A.

1986-01-01

To explain the observed nitrogen distributions in thermally nitridated SiO2 films, a kinetic model is proposed in which the nitridation process is simulated, using the first-order chemical kinetics and Arrhenius dependence of the diffusion and reaction rates on temperature. The calculations show that initially, as the substrate reacts with diffusing nitrogen, a nitrogen-rich oxynitride forms at the SiO2-Si interface, while at nitridation temperatures above 1000 C, an oxygen-rich oxynitride subsequently forms at the interface, due to reaction of the substrate with an increasingly concentrated oxygen displaced by the slower nitridation of the SiO2. This sequence of events results in a nitrogen distribution in which the peak of the interfacial nitrogen concentration occurs away from the interface. The results are compared with the observed nitrogen distribution. The calculated results have correctly predicted the positions of the interfacial nitrogen peaks at the temperatures of 800, 1000, and 1150 C. To account for the observed width of the interfacial nitrogen distribution, it was found necessary to include in the simulations the effect of interfacial strain.

Enhanced Electroluminescence from Silicon Quantum Dots Embedded in Silicon Nitride Thin Films Coupled with Gold Nanoparticles in Light Emitting Devices

PubMed Central

Muñoz-Rosas, Ana Luz; Alonso-Huitrón, Juan Carlos

2018-01-01

Nowadays, the use of plasmonic metal layers to improve the photonic emission characteristics of several semiconductor quantum dots is a booming tool. In this work, we report the use of silicon quantum dots (SiQDs) embedded in a silicon nitride thin film coupled with an ultra-thin gold film (AuNPs) to fabricate light emitting devices. We used the remote plasma enhanced chemical vapor deposition technique (RPECVD) in order to grow two types of silicon nitride thin films. One with an almost stoichiometric composition, acting as non-radiative spacer; the other one, with a silicon excess in its chemical composition, which causes the formation of silicon quantum dots imbibed in the silicon nitride thin film. The ultra-thin gold film was deposited by the direct current (DC)-sputtering technique, and an aluminum doped zinc oxide thin film (AZO) which was deposited by means of ultrasonic spray pyrolysis, plays the role of the ohmic metal-like electrode. We found that there is a maximum electroluminescence (EL) enhancement when the appropriate AuNPs-spacer-SiQDs configuration is used. This EL is achieved at a moderate turn-on voltage of 11 V, and the EL enhancement is around four times bigger than the photoluminescence (PL) enhancement of the same AuNPs-spacer-SiQDs configuration. From our experimental results, we surmise that EL enhancement may indeed be due to a plasmonic coupling. This kind of silicon-based LEDs has the potential for technology transfer. PMID:29565267

Investigation of Coatings for Langmuir Probes in an Oxygen-Rich Space Environment

NASA Astrophysics Data System (ADS)

Samaniego, J. I.; Wang, X.; Andersson, L.; Malaspina, D.; Ergun, R.; Horanyi, M.

2017-12-01

The surface properties of the Langmuir probes, such as the one on the MAVEN mission, will change after exposure to upper planetary atmospheres where high concentrations of atomic oxygen and other oxidizing compounds are present. TiN (Titanium Nitride) or DAG (a resin based graphite dispersion) are the most common coatings for current Langmuir probes, yet both of these coatings pose issues when exposed to oxygen-rich space environment. TiN showed reduced surface conductivity while the DAG layers erode with exposure to oxygen. It is known that Iridium (Ir) and Rhenium (Rh) are difficult to oxidize and maintain high conductivity even in their oxidized forms, suggesting them to be good candidates for probe coatings. Oxidation of most metals creates a resistive layer on the surface of the probe that will affect the amount of current being collected at a given voltage during the probe sweep and therefore affect the accuracy of plasma parameters determined by the Langmuir probe (e.g. density, temperature). We present the results of the oxidation effect on the current-voltage curves (I-V curves) and therefore the resulting measured plasma parameters of Ir and Rh wire probes compared with other control metals and coatings (Cu, Ni, TiN) in controlled plasma environments. The oxidation process is performed in an oxygen plasma chamber in which both O+ and O2+ are created and accelerated toward the probes with energies < 10 eV. An argon plasma chamber is used to compare the probe's I-V curves before and after the oxidation process. Our preliminary results indicate that iridium shows the least effect of oxidation on the probe measurements. The second objective of this study is to identify methods that can be used in orbit to clean the surface of Langmuir probes to minimize the effect of exposure to oxidizing compounds.

Nitride Fuel Development Using Cryo-process Technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

O'Brien, Brandi M; Windes, William E

A new cryo-process technique has been developed for the fabrication of advanced fuel for nuclear systems. The process uses a new cryo-processing technique whereby small, porous microspheres (<2000 µm) are formed from sub-micron oxide powder. A simple aqueous particle slurry of oxide powder is pumped through a microsphere generator consisting of a vibrating needle with controlled amplitude and frequency. As the water-based droplets are formed and pass through the microsphere generator they are frozen in a bath of liquid nitrogen and promptly vacuum freeze-dried to remove the water. The resulting porous microspheres consist of half micron sized oxide particles heldmore » together by electrostatic forces and mechanical interlocking of the particles. Oxide powder microspheres ranging from 750 µm to 2000 µm are then converted into a nitride form using a high temperature fluidized particle bed. Carbon black can be added to the oxide powder before microsphere formation to augment the carbothermic reaction during conversion to a nitride. Also, the addition of ethyl alcohol to the aqueous slurry reduces the surface tension energy of the droplets resulting in even smaller droplets forming in the microsphere generator. Initial results from this new process indicate a lower impurity contamination in the final nitrides due to the single feed stream of particles, material handling and conversion are greatly simplified, a minimum of waste and personnel exposure are anticipated, and finally the conversion kinetics may be greatly increased because of the small oxide powder size (sub-micron) forming the porous microsphere. Thus far the fabrication process has been successful in demonstrating all of these improvements with surrogate ZrO2 powder. Further tests will be conducted in the future using the technique on UO2 powders.« less

Process Development of Gallium Nitride Phosphide Core-Shell Nanowire Array Solar Cell

NASA Astrophysics Data System (ADS)

Chuang, Chen

Dilute Nitride GaNP is a promising materials for opto-electronic applications due to its band gap tunability. The efficiency of GaNxP1-x /GaNyP1-y core-shell nanowire solar cell (NWSC) is expected to reach as high as 44% by 1% N and 9% N in the core and shell, respectively. By developing such high efficiency NWSCs on silicon substrate, a further reduction of the cost of solar photovoltaic can be further reduced to 61$/MWh, which is competitive to levelized cost of electricity (LCOE) of fossil fuels. Therefore, a suitable NWSC structure and fabrication process need to be developed to achieve this promising NWSC. This thesis is devoted to the study on the development of fabrication process of GaNxP 1-x/GaNyP1-y core-shell Nanowire solar cell. The thesis is divided into two major parts. In the first parts, previously grown GaP/GaNyP1-y core-shell nanowire samples are used to develop the fabrication process of Gallium Nitride Phosphide nanowire solar cell. The design for nanowire arrays, passivation layer, polymeric filler spacer, transparent col- lecting layer and metal contact are discussed and fabricated. The property of these NWSCs are also characterized to point out the future development of Gal- lium Nitride Phosphide NWSC. In the second part, a nano-hole template made by nanosphere lithography is studied for selective area growth of nanowires to improve the structure of core-shell NWSC. The fabrication process of nano-hole templates and the results are presented. To have a consistent features of nano-hole tem- plate, the Taguchi Method is used to optimize the fabrication process of nano-hole templates.

Tunable Patch Antennas Using Microelectromechanical Systems

DTIC Science & Technology

2011-05-11

Figure 28, was selected as most suitable to this application. MetalMUMPs is a surface micromachining process with polysilicon , silicon nitride, nickel...yields. MEMS Variable Capacitor Design The MEMS capacitors reported here were an original design that features nickel and polysilicon layers as...the movable plates of a variable parallel plate capacitor. The polysilicon layer was embedded in silicon nitride for electrical isolation and suspended