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At least 37 records · Page 2

Growth of zeolite crystals in the microgravity environment of space

Zeolites are hydrated, crystalline aluminosilicates with alkali and alkaline earth metals substituted into cation vacancies (Equation A) M(sub 2/n) 0-Al203-XSi02-YH20 A They have a uniform internal channel system which makes them ideal for use as catalysts and adsorbents. Presently zeolite materials constitute a 1-2 mi 11 ion dol lar/year business. Typically zeolite crystals are 3-8 µm along their characteristic dimension (e.g., edge). Larger zeolite crystals are desirable. Large crystals will allow more detail characterization of their complex crystal structures. Also, they will help improve reactor performance, may be used as membrane separators, and they should enhance basic studies in molecular diffusion in zeolites. Large zeolite crystals have been produced (100-200 µm) ; however, they have taken restrictively long times to grow. It has been proposed if the rate of nucleation or in some other way the number of nuclei can be lowered, fewer, larger crystals will be formed. provide an ideal condition to achieve rapid growth of large zeolite crystals (e.g., >l00 µm). Since settling crystals are believed to cause secondary nucleation, by limiting crystal movement by suspension in the zero gravity environment, fewer crystals will form, but they will grow larger. The objective of the project is to establish if large zeolite crystals can be formed rapidly in space.

A. Sacco, Jr.↗

Development of SiC Large Tapered Crystal Growth

Majority of very large potential benefits of wide band gap semiconductor power electronics have NOT been realized due in large part to high cost and high defect density of commercial wafers. Despite 20 years of development, present SiC wafer growth approach is yet to deliver majority of SiC's inherent performance and cost benefits to power systems. Commercial SiC power devices are significantly de-rated in order to function reliably due to the adverse effects of SiC crystal dislocation defects (thousands per sq cm) in the SiC wafer.

Neudeck, Phil↗

Method of making macrocrystalline or single crystal semiconductor material

A macrocrystalline or single crystal semiconductive material is formed from a primary substrate including a single crystal or several very large crystals of a relatively low melting material. This primary substrate is deposited on a base such as steel or ceramic, and it may be formed from such metals as zinc, cadmium, germanium, aluminum, tin, lead, copper, brass, magnesium silicide, or magnesium stannide. These materials generally have a melting point below about 1000 C and form on the base crystals the size of fingernails or greater. The primary substrate has an epitaxial relationship with a subsequently applied layer of material, and because of this epitaxial relationship, the material deposited on the primary substrate will have essentially the same crystal size as the crystals in the primary substrate. If required, successive layers are formed, each of a material which has an epitaxial relationship with the previously deposited layer, until a layer is formed which has an epitaxial relationship with the semiconductive material. This layer is referred to as the epitaxial substrate, and its crystals serve as sites for the growth of large crystals of semiconductive material. The primary substrate is passivated to remove or otherwise convert it into a stable or nonreactive state prior to deposition of the seconductive material.

Shlichta, P. J.↗

Development of SiC Large Tapered Crystal Growth

Research Focus Area: Power Electronics, Temperature Tolerant Devices. Demonstrate initial feasibility of totally new "Large Tapered Crystal" (LTC) process for growing vastly improved large-diameter wide-band gap wafers. Addresses Targets: The goal of this research is to experimentally investigate and demonstrate feasibility of the key unproven LTC growth processes in SiC. Laser-assisted growth of long SiC fiber seeds. Radial epitaxial growth enlargement of seeds into large SiC boules. Uniqueness and Impacts open a new technology path to large-diameter SiC and GaN wafers with 1000-fold defect density improvement at 2-4 fold lower cost. Leapfrog improvement in wide band gap power device capability and cost.

Neudeck, Phil↗

Characterization of physio-chemical properties of polymeric and electrochemical materials for aerospace flight

Sealed nickel cadmium cells having undergone a large number of cycles were discharged using the Hg/HgO reference electrode. The negative electrode exhibited the second plateau. SEM of negative plates of such cells show clusters of large crystals of cadmium hydroxide. These large crystals on the negative plates disappear after continuous overcharging in flooded cells. Atomic Absorption Spectroscopy and standard wet chemical methods are being used to determine the cell materials viz: nickel, cadmium, cobalt, potassum and carbonate. The anodes and cathodes are analyzed after careful examination and the condition of the separator material is evaluated.

Rock, M.↗

Second Plateau Voltage in Nickel-cadmium Cells

Sealed nickel cadmium cells having large number of cycles on them are discharged using Hg/HgO reference electrode. The negative electrode exhibits the second plateau. A SEM of negative plates of such cells show a number of large crystals of cadmium hydroxide. The large crystals on the negative plates disappear after continuous overcharging in flooded cells.

Vasanth, K. L.↗

BaGa{sub 2}GeX{sub 6}(X=S, Se): New mid-IR nonlinear optical crystals with large band gaps

New middle infrared nonlinear optical crystals of BaGa{sub 2}GeX{sub 6}(X=S, Se) have been synthesized. The structures of both BaGa{sub 2}GeS{sub 6} and BaGa{sub 2}GeSe{sub 6} were found to be isomorphous exhibiting a three-dimensional framework constructed by the parallel alignment of Ga or Ge tetrahedron groups along the c-aix. The ultraviolet transmittance spectrum indicates the short-wavelength absorption edges of BaGa{sub 2}GeS{sub 6} and BaGa{sub 2}GeSe{sub 6} are 380 nm and 440 nm, respectively. The IR transmittance spectrum shows that the absorption edge of the BaGa{sub 2}GeS{sub 6} crystal is 13.7 {mu}m. Second-harmonic generation of the powder samples was measured with a 2.05 {mu}m laser using the Kurtz and Perry technique, which showed that BaGa{sub 2}GeS{sub 6} and BaGa{sub 2}GeSe{sub 6} are phase-matched materials, and their measured SHG coefficient is {approx}2.1 and {approx}3.5 times as large as the coefficient of AgGaS{sub 2}, or 26.3 pm/V and 43.7 pm/V. - Graphical abstract: The structure of BGGS viewed along the a and c axis and an as-grown crystal. Highlights: Black-Right-Pointing-Pointer Mid-IR NLO crystals of BaGa{sub 2}GeX{sub 6}(X=S, Se) with wide band-gap have been discovered. Black-Right-Pointing-Pointer The structures were constructed by the parallel alignment of Ga or Ge tetrahedra. Black-Right-Pointing-Pointer They are phase-matchable material with their SHG coefficient of 26.3 and 43.7 pm/V.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The specific light output of cesium iodide crystals

Large area ion chambers for a high energy cosmic ray experiment, scintillating plastic fibers as light pipes for a cosmic ray hodoscope, and an evaluation of clad scintillating light pipes were considered.

Gregory, J. C.↗

Three-dimensional photonic crystals by large-area membrane stacking

We designed and analyzed a “mesh-stack” three-dimensional photonic crystal of a 12.4% bandgap with a dielectric constant ratio of 12:1. The mesh-stack consists of four offset identical square-lattice air-hole patterned membranes in each vertical period that is equal to the in-plane period of the square lattice. This design is fully compatible with the membrane-stacking fabrication method, which is based on alignment and stacking of large-area single-crystal membranes containing engineered defects. A bandgap greater than 10% is preserved as long as the membranes are subjected to in-plane misalignment less than 3% of the square period. By introducing a linear defect with a nonsymmorphic symmetry into the mesh-stack, we achieved a single-mode waveguide over a wide bandwidth.

36 MATERIALS SCIENCE↗

Chemical Vapor Synthesis of Titanium Aluminides by Reaction of Aluminum Subchloride and Titanium Tetrachloride

A new process for developing titanium aluminides (TiAls) using chemical vapor synthesis was investigated in a laboratory experiment. Aluminum subchloride (AlCl) was used as the reducing agent in the reaction with TiCl{sub 4} and the source of aluminum for Ti-Al alloy. Two types of products, with large crystals and fine particles, were fabricated. The large crystals were determined to be TiAl, with small amounts of Ti and Ti{sub 3}Al phases. The composition of fine particles, on the other hand, varied in wide range.

36 MATERIALS SCIENCE↗

Solar furnace satellite for large diameter crystal growth in space

Investigators worldwide are preparing experiments to test the influence of low gravity found in space on the growth of many crystalline materials. However, power limitations prevent existing space crystal growth furnaces from being able to process samples any larger than about 2 cm, and in addition, the background microgravity levels found on the Space Shuttle are not low enough to significantly benefit samples much larger than 2 cm. This paper describes a novel concept of a free-flying platform utilizing well-established solar furnace technology to enable materials processing in space experiments on large-diameter crystals. The conceptual design of this Solar Furnace Satellite is described along with its operational scenario and the anticipated g levels.

Overfelt, Tony↗

Projection x-ray topography system at 1-BM x-ray optics test beamline at the advanced photon source

Projection X-ray topography of single crystals is a classic technique for the evaluation of intrinsic crystal quality of large crystals. In this technique a crystal sample and an area detector (e.g., X-ray film) collecting intensity of a chosen crystallographic reflection are translated simultaneously across an X-ray beam collimated in the diffraction scattering plane (e.g., [1, 2]). A bending magnet beamline of a third-generation synchrotron source delivering x-ray beam with a large horizontal divergence, and therefore, a large horizontal beam size at a crystal sample position offers an opportunity to obtain X-ray topographs of large crystalline samples (e.g., 6-inch wafers) in just a few exposures. Here we report projection X-ray topography system implemented recently at 1-BM beamline of the Advanced Photon Source. A selected X-ray topograph of a 6-inch wafer of 4H-SiC illustrates capabilities and limitations of the technique.

43 PARTICLE ACCELERATORS↗

Make Selenium Reactive Again: Activating Elemental Selenium for Synthesis of Metal Selenides Ranging from Nanocrystals to Large Single Crystals

The inertness of elemental selenium is a significant obstacle in the synthesis of selenium-containing materials at low reaction temperatures. Over the years, several recipes have been developed to overcome this hurdle; however, most of the methods are associated with the use of highly toxic, expensive, and environmentally harmful reagents. As such, there is an increasing demand for the design of cheap, stable, and nontoxic reactive selenium precursors usable in the low-temperature synthesis of transition metal selenides with vast applications in nanotechnology, thermoelectrics, and superconductors. Herein, a novel synthetic route has been developed for activating elemental selenium by using a solvothermal approach. By comprehensive 77 Se NMR, Raman, and infrared spectroscopies and gas chromatography–mass spectrometry, we show that the activated Se solution contained HSe – , [Se–Se] 2– , and Se 2– ions, as well as dialkyl selenide (R 2 Se) and dialkyl diselenide (R–Se–Se–R) species in dynamic equilibrium. This also corresponded to the first observation of naked Se 2 2– in solution. The versatility of the developed Se precursor was demonstrated by the successful synthesis of (i) the polycrystalline room-temperature modification of the β-Ag 2 Se thermoelectric material; (ii) large single crystals of superconducting β-FeSe; (iii) CdSe nanocrystals with different particle sizes (3–10 nm); (iv) nanosheets of PtSe 2 ; and (v) mono- and dibenzyl selenides and diselenides at room temperature. In conclusion, The simplicity and diversity of the developed Se activation method holds promise for applied and fundamental research.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unraveling the convoluted and dynamic interphasial mechanisms on Li metal anode

Accurate understanding of the chemistry of solid-electrolyte interphase (SEI) is key to developing new electrolytes for high-energy batteries using lithium metal (Li-0) anodes(1). SEI is generally believed to be formed by the reactions between Li-0 and electrolyte(2,3). However, our new study shows this is not the whole story. Through synchrotron-based X-ray diffraction and pair distribution function analysis, we reveal a much more convoluted formation mechanism of SEI, which receives considerable contributions from electrolyte, cathode, moisture and native surface species on Li-0, with highly dynamic nature during cycling. Using isotope labelling, we traced the origin of LiH to electrolyte solvent, moisture and a new source: the native surface species (LiOH) on pristine Li-0. When lithium accessibility is very limited as in the case of anode-free cells, LiOH develops into plate-shaped large crystals during cycling. Alternatively, when the lithium source is abundant, as in the case of Li||NMC811 cells, LiOH reacts with Li-0 to form LiH and Li2O. While the desired anion-derived LiF-rich SEI is typically found in the concentrated electrolytes or their derivatives, we found it can also be formed in low-concentration electrolyte via the crosstalk effect, emphasizing the importance of formation cycle protocol and opening up opportunities for low-cost electrolyte development.

Polzin, Bryant J.↗

A Test of Macromolecular Crystallization in Microgravity: Large, Well-Ordered Insulin Crystals

Crystals of insulin grown in microgravity on space shuttle mission STS-95 were extremely well-ordered and unusually large (many > 2 mm). The physical characteristics of six microgravity and six earth-grown crystals were examined by X-ray analysis employing superfine f slicing and unfocused synchrotron radiation. This experimental setup allowed hundreds of reflections to be precisely examined for each crystal in a short period of time. The microgravity crystals were on average 34 times larger, had 7 times lower mosaicity, had 54 times higher reflection peak heights and diffracted to significantly higher resolution than their earth grown counterparts. A single mosaic domain model could account for reflections in microgravity crystals whereas reflections from earth crystals required a model with multiple mosaic domains. This statistically significant and unbiased characterization indicates that the microgravity environment was useful for the improvement of crystal growth and resultant diffraction quality in insulin crystals and may be similarly useful for macromolecular crystals in general.

Borgstahl, Gloria E. O.↗

Electrostatic Stabilization Of Growing Protein Crystals

Proposed technique produces large crystals in compact, economical apparatus. Report presents concept for supporting protein crystals during growth in microgravity. Yields crystals larger and more-nearly perfect than those grown on Earth. Combines best features of sandwich-drop and electrostatic-levitation methods of support. Drop of protein solution inserted between pair of glass or plastic plates, as in sandwich-drop-support method. Electrostatically charged ring confines drop laterally and shapes it, as in electrostatic technique. Apparatus also made to accommodate several drops simultaneously between same pair of supporting plates. Drops can be inserted and crystals removed through ducts in plates.

Shlichta, Paul J.↗