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At least 19 records

Elevated temperature compressive properties of reaction milled NiAl-AlN and Zr-doped NiAl-AlN composites

Previous studies of a single lot of NiAl powder which had been ground under high intensity conditions in liquid nitrogen (cryomilling) indicated that this processing leads to a high strength, elevated temperature NiAl-AlN composite. Because this was the first known example of the use of the reaction milling process to produce a high temperature composite, the reproducibility of this technique was unknown. Two additional lots of NIAl powder and a lot of a Zr-doped NiAl powder have been cryomilled, and analyses indicate that AlN was formed within a NiAl matrix in all three cases. Compression testing between 1200 K and 1400 K has shown that the deformation resistance of these heats is similar to that of the first lot of NiAl-AlN; thus cryomilling can improve the creep resistance of NiAl by a factor of six. Based on this work, it is concluded that cryomilling of NiAl powder to form high temperature, high strength NiAl-AlN composites is a reproducible process.

Whittenberger, J. D.↗

Theoretical spectrum of AlN

Theoretical spectroscopic constants and radiative lifetimes are presented for the low-lying electronic states of AlN and AlN(+). The ground state of AlN is predicted to be X 3Pi, in agreement with earlier theoretical calculations, but the A 3Pi- state is extremely low-lying. The near degeneracy of these states is analogous to the situation for Al2 and implies that sigma and pi bonds are of nearly equal strength. The 3Pi - 3Pi AlN band system observed in emission is assigned as the C 3Pi - X 3Pi transition. The C 3Pi radiative lifetime is estimated as 151, 163, and 175 ns for v-prime = 0, 1, 2 respectively. These lifetimes may be significantly shortened by dissociation by the (1) 5Pi stated. The calculated D(e) of 2.35 eV for the ground state is about half that of the isovalent BN molecule. Thus the bonding in AlN is significantly weaker than for BN owing to the smaller overlaps of the valence orbitals.

Langhoff, Stephen R.↗

Cyclic oxidation resistance of a reaction milled NiAl-AlN composite

Based upon recent mechanical property tests a NiAl-AlN composite produced by cryomilling has very attractive high temperature strength. This paper focuses on the oxidation resistance of the NiAl-AlN composite at 1473 and 1573 K as compared to that of Ni-47Al-0.15Zr, one of the most oxidation resistant intermetallics. The results of cyclic oxidation tests show that the NiAl-AlN composite has excellent properties although not quite as good as those of Ni-47Al-0.15Zr. The onset of failure of the NiAl-AlN was unique in that it was not accompanied by a change in scale composition from alumina to less protective oxides. Failure in the composite appears to be related to the entrapment of AlN particles within the alumina scale.

Lowell, Carl E.↗

Characteristics of an Elevated Temperature ALN Particulate Reinforced NiAl

High energy milling of NiAl in liquid nitrogen (cryomilling) leads to the formation of a discontinuously AlN particle reinforced aluminide which has shown good potential as a high strength oxidation resistant material. Experiments have demonstrated that cryomilling is repeatable, and materials with reproducible chemistries and mechanical properties result. Furthermore, it is possible to vary the AlN content through control of the milling parameters. Tensile creep as well as compressive creep testing has been undertaken on a lot of NiAl-AlN. While this material is weaker in tension than compression, the tensile strength is respectable: for example, the creep rupture life exceeds 2700 h at 1300 K, 50 MPa. Heat treatment of the particulate reinforced aluminide at 1600 K promotes AlN growth which weakens the material but does not change the deformation mechanism. Cyclic oxidation testing of lots of NiAl-AlN which were cryomilled with and without yttria reveal that Y2O3 promotes better oxidation resistance. However, the presence or absence of yttria had no affect on the mechanical properties.

Whittenberger, J. D.↗

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

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.

Kaul, Anupama↗

NiAl-base composite containing high volume fraction of AlN for advanced engines

A particulate reinforced NiAl-AlN composite alloy has a NiAl matrix and greater than about 13 volume percent fine particles of AlN within the matrix. The particles preferably have a diameter from about 15 nanometers to about 50 nanometers. The particulate reinforced NiAl-AlN composite alloy may be prepared by cryomilling prealloyed NiAl in liquid nitrogen using grinding media having a diameter of from about 2 to 6 mm at an impeller speed of from about 450 RPM to about 800 RPM. The cryomilling may be done for a duration of from about 4 hours to about 20 hours to obtain a cryomilled powder. The cryomilled powder may be consolidated to form the particulate reinforced NiAl-AlN composite alloy. The particulate reinforced alloy can further include a toughening alloy. The toughening alloy may include NiCrAlY, FeCrAlY, and FeAl.

Hebsur, Mohan↗

The Oxidation of AlN in Dry and Wet Oxygen

The oxidation kinetics of AlN containing 3.5 wt% Y2O3 were studied by thermogravimetric analysis in dry oxygen and 10% H2O/balance oxygen at temperatures between 1000 and 1200 C for times between 48 and 100 h. The oxidation kinetics for AlN in dry oxygen were parabolic and of approximately the same magnitude and temperature dependence as other alumina forming materials. In this case, diffusion of oxygen and/or aluminum through the alumina scale is the rate limiting mechanism. The oxidation kinetics for AlN in wet oxygen were nearly linear and much more rapid than rates observed in dry oxygen. Numerous micropores were observed in the alumina formed on AIN in wet oxygen. These pores provide a fast path for oxygen transport. The linear kinetics observed in this case suggest that the interface reaction rate of AlN with wet oxygen is the oxidation rate limiting step.

Opila, Elizabeth↗

Nial-base composite containing high volume fraction of AlN for advanced engines

A particulate reinforced NiAl-AlN composite alloy has a NiAl matrix and greater than about 13 volume percent fine particles of AlN within the matrix. The particles preferably have a diameter from about 15 nanometers to about 50 nanometers. The particulate reinforced NiAl-AlN composite alloy may be prepared by cryomilling prealloyed NiAl in liquid nitrogen using grinding media having a diameter of from about 2 mm to about 6 mm at an impeller speed of from about 450 RPM to about 800 RPM. The cryomilling may be done for a duration of from about 4 hours to about 20 hours to obtain a cryomilled powder. The cryomilled powder may be consolidated to form the particulate reinforced NiAl-AlN composite alloy. The particulate reinforced alloy can further include a toughening alloy. The toughening alloy may include NiCrAlY, FeCrAY and FeAl.

Hebsur, Mohan G.↗

CVD of SiC and AlN using cyclic organometallic precursors

The use of cyclic organometallic molecules as single-source MOCVD precursors is illustrated by means of examples taken from our recent work on AlN and SiC deposition, with particular focus on SiC. Molecules containing (AlN)3 and (SiC)2 rings as the 'core structure' were employed as the source materials for these studies. The organoaluminum amide, (Me2AlNH2)3, was used as the AlN source and has been studied in a molecular beam sampling apparatus in order to determine the gas phase species present in a hot-wall CVD reactor environment. In the case of SiC CVD, a series of disilacyclobutanes (Si(XX')CH2)2 (with X and X' = H, CH3, and CH2SiH2CH3), were examined in a cold-wall, hot-stage CVD reactor in order to compare their relative reactivities and prospective utility as single-source CVD precursors. The parent compound, disilacyclobutane, (SiH2CH2)2, was found to exhibit the lowest deposition temperature (ca. 670 C) and to yield the highest purity SiC films. This precursor gave a highly textured, polycrystalline film on the Si(100) substrates.

Interrante, L. V.↗

A Chemical and Structural Study of the AlN-Si Interface

The growth of low defect density heteroepitaxial AlN has great implications for optoelectronic and high power devices since the AlN can be used either as device material or as a buffer layer for the overgrowth of other group-III nitrides. In this work, the results of transmission electron microscopy (TEM) involving both high resolution imaging and electron energy loss spectroscopy (EELS) of AlN/Si layers is reported and the relationship between Si-Al-N interactions and the misorientation of AlN nuclei is elucidated.

epitaxial optoelectronic silicon gallium nitride↗

Development of Field-Controlled Smart Optic Materials (ScN, AlN) with Rare Earth Dopants

The purpose of this investigation is to develop the fundamental materials and fabrication technology for field-controlled spectrally active optics that are essential for industry, NASA, and DOD applications such as: membrane optics, filters for LIDARs, windows for sensors, telescopes, spectroscopes, cameras, flat-panel displays, etc. ScN and AlN thin films were fabricated on c-axis Sapphire (0001) or quartz substrate with the RF and DC magnetron sputtering. The crystal structure of AlN in fcc (rocksalt) and hcp (wurtzite) were controlled. Advanced electrical characterizations were performed, including I-V and Hall Effect Measurement. ScN film has a free carrier density of 5.8 x 10(exp 20)/per cubic centimeter and a conductivity of 1.1 x 10(exp 3) per centimeter. The background ntype conductivity of as-grown ScN has enough free electrons that can readily interact with the photons. The high density of free electrons and relatively low mobility indicate that these films contain a high level of shallow donors as well as deep levels. Also, the UV-Vis spectrum of ScN and AlN thin films with rare earth elements (Er or Ho) were measured at room temperature. Their optical band gaps were estimated to be about 2.33eV and 2.24eV, respectively, which are obviously smaller than that of undoped thin film ScN (2.4eV). The red-shifted absorption onset gives direct evidence for the decrease of band gap (Eg) and the energy broadening of valence band states are attributable to the doping. As the doped elements enter the ScN crystal lattices, the localized band edge states form at the doped sites with a reduction of Eg. Using a variable angle spectroscopic ellipsometer, the decrease in refractive index with applied field is observed with a smaller shift in absorption coefficient.

Kim, Hyun-Jung↗

1300 K compressive properties of a reaction milled NiAl-AlN composites

When B2 crystal-structure nickel aluminide is subjected to high-intensity mechanical ball milling in a liquid nitrogen bath, or 'cryomilling', an NiAl composite is obtained which contains about 10 vol pct AlN particles. This composition arises from the incorporation of N during cryomilling; during subsequent thermomechanical processing, the N reacts with Al. While compressive testing of extruded or isostatically pressed specimens at 1300 K indicated that strength at relatively fast strain rates is slightly dependent on consolidation method, slower strain rates indicate no clear dependency on densification technique: four different consolidation methods were found to yield similar creep strengths. The creep properties of NiAl-AlN are similar to those of the single-crystal Ni-base superalloy NASAIR 100.

Whittenberger, J. Daniel↗

A Microstructural Analysis of Orientation Variation in Epitaxial AlN on Si, Its Probable Origin, and Effect on Subsequent GaN Growth

A structural examination of aluminum nitride growth on [111] silicon was carried out using transmission electron microscopy. Electron diffraction indicates that the basal planes of the wurtzitic overlayer mimic the orientation of the close-packed planes of the substrate. However, considerable, random rotation in the basal plane and random out-of-plane tilts were evident. This article examines these issues with a structural examination of AlN and GaN/AlN on silicon and compares the findings to those reported in the literature.

GaN AlN Si epitaxial aluminum gallium nitride↗

Waveguide-coupled resonator filters on AlN on silicon

In the effort to continually reduce the size and cost of wireless communications products the level of integration has improved dramatically in recent years. In order to reduce future generations of wireless systems to single chip form, there is a need for on-chip filtering capabilities. In this paper, the first report of an experimental waveguide-coupled resonator filter for cellular radio applications is presented. Measured results indicate a typical insertion loss of 26 dB at a center frequency of 132 MHz using a 2 um AlN film on (001) less than 110 greater than Si. In addition, a laser probe analysis has been conducted and a theoretical analysis of the first order reflection coefficients is presented.

Liaw, H. M.↗

Coating MCPs with AlN and GaN

A development effort underway at the time of reporting the information for this article is devoted to increasing the sensitivity of microchannel plates (MCPs) as detectors of photons and ions by coating the MCPs with nitrides of elements in period III of the periodic table. Conventional MCPs are relatively insensitive to slowly moving, large-mass ions for example, ions of biomolecules under analysis in mass spectrometers. The idea underlying this development is to coat an MCP to reduce its work function (decrease its electron affinity) in order to increase both (1) the emission of electrons in response to impingement of low-energy, large-mass ions and (2) the multiplying effect of secondary electron emission. Of particular interest as coating materials having appropriately low or even negative electron affinities are gallium nitride, aluminum nitride, and ternary alloys of general composition Al(x)Ga(1-x)N (where 0<x<1). These materials exhibit attractively high degrees of chemical, mechanical, and thermal stability plus acceptably high resistance to sputtering. The electron-excitation cross sections of these materials are expected to exceed those of several other materials (including diamond) that are, variously, in use or under development for the same purpose. Moreover, by doping these materials with silicon, one can render them partly electrically conductive, thereby suppressing the undesired accumulation of electric charge that could otherwise occur during bombardment by ions. For experiments, thin films of AlN and GaN both undoped and doped with Si were deposited on commercial MCPs by radio-frequency molecular-beam epitaxy (also known as plasma-assisted molecular-beam epitaxy) at temperatures <200 C. This deposition technique is particularly suitable because (1) MCPs cannot withstand the higher deposition-substrate temperatures used to decompose constituent compounds in some other deposition techniques and (2) in this technique, the constituent Al, Ga, and N are supplied in elemental form, so that there is no need for thermal decomposition at the substrate surface. The nitride films thus formed were, variously, amorphous or polycrystalline. The nitride films were coated with surface layers of gold <100 thick. The MCPs were tested in a standard configuration in which the output stage of a first MCP was coupled to the input stage of a second MCP. Each pair of MCPs was mounted in a standard holder that included front and back contact rings and an anode for collecting the output electrons of the second MCP. The MCP pairs were biased at potentials between 1.7 and 1.9 kV, and count rates measured after preamplification and discrimination. To enable a direct comparison, in one pair, the second MCP was uncoated while the first MCP was coated over half its surface. The coated and uncoated sides of the half-coated MCP were exposed to fluxes of argon ions at kinetic energies of 1.0 and 0.5 keV. At 1.0 keV, the count rate for the coated side was about 2.3 times greater than that for the uncoated side; at 0.5 keV, the count rate for the coated side was about 1.8 times greater than that for the uncoated side.

Bensaoula, Abdelhakim↗

High Temperature W-band Complex Permittivity Measurements of Thermally Cycled Ceramic-Metal Composites: AlN:Mo with 0.25 vol% to 4.0 vol% Mo from 25 °C to 1000 °C in Air

An apparatus for measuring the W-band (75-110GHz) complex permittivity of dielectrics at 1000 °C was developed. This apparatus allows for measurements at approximately twice the temperature of previously published high temperature free-space measurement systems while maintaining similar precision. Challenges were addressed related to high temperature measurements, including temperature uniformity, the accuracy of temperature measurements, and preventing temperature related changes to mm-wave measurement systems. The details of complex permittivity extraction from the measured S-parameters are discussed. Sources of error related to permittivity measurement and mathematical models were identified and are discussed in detail herein. Thermally-cycled, mm-wave absorbing, aluminum nitride ceramic composites containing varying levels of molybdenum additives were measured over the range of 25-1000 °C. These measurements were compared to the same composites before thermal cycling. It was found that ceramic composites are largely stable after thermal cycling in terms of dielectric properties despite the presence of visible surface modifications.

Zane W Cohick↗

Optical and electrical characterizations of laser-chemical-vapor-deposited aluminum oxynitride films

Composition-dependent optical and electrical properties of L-CVD (Al2O3)1-c-(AlN)c composite films are examined. The optical properties exhibit a continuous change from Al2O3 to AlN with increasing value of the composition parameter c from zero to one. There is a critical concentration value of about 0.3 below and above which Al2O3- and AlN-like optical properties are observed. The impurity absorption regions are 5.1-6.7 eV for Al2O32 and 4.6-6.0 for AlN, while the energy gap is about 6.7 eV for Al2O3 and 6.0 eV for AlN. The electrical properties of Al-insulator n-Si MIS structures display externally programmable states when bulk-controlled electron emission occurs from the traps. In the high-field region a persistent polarization field is established within the insulator. C-V characteristics of the samples are more sensitive to the concentration factor c than the I-V characteristics. A large clockwise hysteresis is observed for AlN, but a smaller counterclockwise one is observed for Al2O3.

Demiryont, H.↗