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NASA NTRS2004

Ordered Nanostructures Made Using Chaperonin Polypeptides

A recently invented method of fabricating periodic or otherwise ordered nanostructures involves the use of chaperonin polypeptides. The method is intended to serve as a potentially superior and less expensive alternative to conventional lithographic methods for use in the patterning steps of the fabrication of diverse objects characterized by features of the order of nanometers. Typical examples of such objects include arrays of quantum dots that would serve as the functional building blocks of future advanced electronic and photonic devices. A chaperonin is a double-ring protein structure having a molecular weight of about 60 plus or minus 5 kilodaltons. In nature, chaperonins are ubiquitous, essential, subcellular structures. Each natural chaperonin molecule comprises 14, 16, or 18 protein subunits, arranged as two stacked rings approximately 16 to 18 nm tall by approximately 15 to 17 nm wide, the exact dimensions depending on the biological species in which it originates. The natural role of chaperonins is unknown, but they are believed to aid in the correct folding of other proteins, by enclosing unfolded proteins and preventing nonspecific aggregation during assembly. What makes chaperonins useful for the purpose of the present method is that under the proper conditions, chaperonin rings assemble themselves into higher-order structures. This method exploits such higher-order structures to define nanoscale devices. The higher-order structures are tailored partly by choice of chemical and physical conditions for assembly and partly by using chaperonins that have been mutated. The mutations are made by established biochemical techniques. The assembly of chaperonin polypeptides into such structures as rings, tubes, filaments, and sheets (two-dimensional crystals) can be regulated chemically. Rings, tubes, and filaments of some chaperonin polypeptides can, for example, function as nano vessels if they are able to absorb, retain, protect, and release gases or chemical reagents, including reagents of medical or pharmaceutical interest. Chemical reagents can be bound in, or released from, such structures under suitable controlled conditions. In an example of a contemplated application, a two-dimensional crystal of chaperonin polypeptides would be formed on a surface of an inorganic substrate and used to form a planar array of nanoparticles or quantum dots. Through genetic engineering of the organisms used to manufacture the chaperonins, specific sites on the chaperonin molecules and, thus, on the two-dimensional crystals can be chemically modified to react in a specific manner so as to favor the deposition of the material of the desired nanoparticles or quantum dots. A mutation that introduces a cysteine residue at the desired sites on a chaperonin of Sulfolobus shibatae was used to form planar arrays of gold nanoparticles (see figure).

Trent, Jonathan↗

NASA NTRS2011

Nakhla: a Martian Meteorite with Indigenous Organic Carbonaceous Features

The Nakhla meteorite possesses discrete, well defined, structurally coherent morphologies of carbonaceous phases present within iddingsite alteration zones. Based upon both isotopic measurements and analysis of organic phases the presence of pre-terrestrial organics is now recognized. Within the microcrystalline layers of Nakhla s iddingsite, discrete clusters of salt crystals are present. These salts are predominantly halite (NaCl) with minor MgCl2 crystals. Some CaSO4, likely gypsum, appears to be partially intergrown with some of the halite. EDX mapping shows discrete C-rich features are interspersed among these crystals. A hollow semi-spherical bowl structure (~ 3 m ) has been identified and analyzed after using a focused ion beam (FIB) to cut a transverse TEM thin section of the feature and the underlying iddingsite. TEM/EDX analysis reveals that the feature is primarily carbonaceous containing C with lesser amounts of Si, S, Ca, Cl, F, Na, and minor Mn and Fe; additionally a small peak consistent with N, which has been previously seen in Nakhla carbonaceous matter, is also present. Selected area electron diffraction (SAED) shows that this C-rich material is amorphous (lacking any long-range crystallographic order) and is not graphite or carbonate. Micro-Raman spectra acquired from the same surface from which the FIB section was extracted demonstrate a typical kerogen-like D and G band structure with a weak absorption peak at 1350 and a stronger peak at 1600/cm. The C-rich feature is intimately associated with both the surrounding halite and underlying iddingsite matrix. Both iddingsite and salts are interpreted as having formed as evaporate assemblages from progressive evaporation of water bodies on Mars. This assemblage, sans the carbonaceous moieties, closely resembles iddingsite alteration features previously described which were interpreted as indigenous Martian assemblages. These distinctive macromolecular carbonaceous structures in Nakhla may represent one of the sources of the high molecular weight organic material previously identified in Nakhla. While we do not speculate on the origin of these unique carbonaceous structures, we note that the significance of such observations is that it may allow us to construct a C-cycle for Mars based on the C chemistry of the Martian meteorites with obvious implications for astrobiology and the prebiotic evolution of Mars. In any case, our observations strongly suggest that organic C exists as micrometersize, discrete structures on Mars.

McKay, D. S.↗

NASA NTRS2000

Stereo Imaging Velocimetry of Mixing Driven by Buoyancy Induced Flow Fields

Mixing of two fluids generated by steady and particularly g-jitter acceleration is fundamental towards the understanding of transport phenomena in a microgravity environment. We propose to carry out flight and ground-based experiments to quantify flow fields due to g-jitter type of accelerations using Stereo Imaging Velocimetry (SIV), and measure the concentration field using laser fluorescence. The understanding of the effects of g-jitter on transport phenomena is of great practical interest to the microgravity community and impacts the design of experiments for the Space Shuttle as well as the International Space Station. The aim of our proposed research is to provide quantitative data to the community on the effects of g-jitter on flow fields due to mixing induced by buoyancy forces. The fundamental phenomenon of mixing occurs in a broad range of materials processing encompassing the growth of opto-electronic materials and semiconductors, (by directional freezing and physical vapor transport), to solution and protein crystal growth. In materials processing of these systems, crystal homogeneity, which is affected by the solutal field distribution, is one of the major issues. The understanding of fluid mixing driven by buoyancy forces, besides its importance as a topic in fundamental science, can contribute towards the understanding of how solutal fields behave under various body forces. The body forces of interest are steady acceleration and g-jitter acceleration as in a Space Shuttle environment or the International Space Station. Since control of the body force is important, the flight experiment will be carried out on a tunable microgravity vibration isolation mount, which will permit us to precisely input the desired forcing function to simulate a range of body forces. To that end, we propose to design a flight experiment that can only be carried out under microgravity conditions to fully exploit the effects of various body forces on fluid mixing. Recent flight experiments, by the P.I. through collaboration with the Canadian Space Agency (STS-85, August 1997), aimed at determining the stability of the interface between two miscible liquids inside an enclosure show that a long liquid column (5 cm) under microgravity isolation conditions can be stable, i.e. the interface remains sharp and vertical over a short time scale; thus transport occurs by molecular mass diffusion. On the other hand, when the two liquids were excited from a controlled vibration source (Microgravity Vibration Isolation Mount) two to four mode large amplitude quasi-stationary waves were observed. The data was limited to CCD recording of the dynamics of the interface between the two fluids. We propose to carry out flight experiments to quantify the dynamics of the flow field using Stereo Imaging Velocimetry and measure the concentration field using laser fluorescence. The results will serve as a basis to understand effects of g-jitter on transport phenomena, in this case mass diffusion. As the measurement of the kinematics of the flow field will shed light on the instability mechanism. The research will allow measurement of the flow field in microgravity environment to prove two hypotheses: (1) Maxwell's hypothesis: finite convection always exists in diffusing systems, and (2) Quasi-stationary waves inside a bounded enclosure in a microgravity environment is generated by Kelvin-Helmholtz instability; resonance of the interface which produces incipient mixing is due to Rayleigh-Taylor instability. The first hypothesis can be used as a benchmark experiment to illustrate diffusive mixing. The second hypothesis will lead to the understanding of g-jitter effects on buoyancy driven flow fields which occur in many situations involving materials processing, and other basic fluid physics phenomena. In addition, the second hypothesis will also provide insight in how Rayleigh-Taylor and Kelvin-Helmholtz instabilities propagate concentration fronts during mixing. Measurement of the flow field using SIV is important because it is the flow field which causes instability at the interface between the two fluids. Mixing driven by buoyancy induced flow fields will be addressed both experimentally and computationally. The experimental effort will address the kinematics of mixing: stretching, transport and chaos. Quantification of the mechanisms of mixing will consists of measuring the flow field using the SIV system at Glenn and capturing the dynamics of the interface, to measure mass transport, using a CCD camera. These experiments will be carried out within the framework of Earth's gravity and g-jitter microgravity acceleration as in a Space Shuttle environment or the International Space Station. The g-jitter will be induced and controlled using a tunable vibration isolation platform to isolate against vibration as well as input periodic and random vibration to the system. The parametric range of the microgravity experiment will be extended from the experiments on STS-85 to investigate higher mode quasi-stationary waves (8 to 12), as well as resonance regions which leads to chaos and turbulence. Ground-based experiments will focus on effects of vibration on stably stratified fluid layers in order to scale for possible scenarios in a microgravity environment. These vibrations will be subjected perpendicular to the concentration field on the ground since the parallel case can only be carried out in a microgravity environment. The concept of dynamical similarity will be applied to tune the experiments as closely as possible to a Space Shuttle environment or the International Space Station. The computational effort will take advantage of the Computational Laboratory at Glenn to corroborate the experimental findings with predictions of the dynamics of the flow field using the codes FLUENT (finite difference based) and FIDAP (finite element based). We will investigate two important cases, single-fluid model to address dilute systems with negligible jump in viscosity and the more general two-fluid model which accounts for finite jump in viscosity. Apart from its microgravity relevance, this experiment is well suited to study dynamics in nonlinear systems.

Duval, W. M. B.↗

NASA NTRS2004

Structure and Dynamics of Freely Suspended Liquid Crystals

Smectic liquid crystals are phases of rod shaped molecules organized into one dimensionally (1 D) periodic arrays of layers, each layer being between one and two molecular lengths thick. In the least ordered smectic phases, the smectics A and C, each layer is a two dimensional (2D) liquid. Additionally there are a variety of more ordered smectic phases having hexatic short range translational order or 2D crystalline or quasi long range translational order within the layers. The inherent fluid-layer structure and low vapor pressure of smectic liquid crystals enables the long term stabilization of freely suspended, single component, layered fluid films as thin as 30A, a single molecular layer. The layering forces the films to be an integral number of smectic layers thick, quantizing their thickness in layer units and forcing a film of a particular number of layers to be physically homogeneous with respect to its layer structure over its entire area. Optical reflectivity enables the precise determination of the number of layers. These ultrathin freely suspended liquid crystal films are structures of fundamental interest in condensed matter and fluid physics. They are the thinnest known stable fluid structures and have the largest surface-to-volume ratio of any stable fluid preparation, making them ideal for the study of the effects of reduced dimensionality on phase behavior and on fluctuation and interface phenomena. Their low vapor pressure and quantized thickness enable the effective use of microgravity to extend the study of basic capillary phenomena to ultrathin fluid films. Freely suspended films have been a wellspring of new LC physics. They have been used to provide unique experimental conditions for the study of condensed phase transitions in two dimensions. They are the only system in which the hexatic has been unambiguously identified as a phase of matter, and the only physical system in which fluctuations of a 2D XY system and Kosterlitz Thouless phase transition has been observed and 2D XY quasi long range order verified. Smectic films have enabled the precise determination of smectic layer electron density and positional fluctuation profiles and have been used to show that the interlayer interactions in antiferroelectric tilted smectics do not extend significantly beyond nearest neighbors. Freely suspended films played a pivotal role in the recent discovery of macroscopic chiral-polar ordering in fluids of achiral molecules. The interactions which are operative in liquid crystals are generally weak in comparison to those in crystalline phases, leading to the facile manipulation of the order in liquid crystals by external agents such as applied fields and surfaces. Effects arising from weak ordering are significantly enhanced in ultrathin free films and filaments, in which the intermolecular coupling is effectively further reduced by loss of neighbors. Over the past four years this research, which we now detail, has produced a host of exciting new discoveries and unexpected results, maintaining the study of freely suspended liquid crystal structures as one of most exciting and fruitful areas of complex fluid physics. In addition, a class of experiments on the behavior of 1D interfaces in 2D films have been pursued with results that point to potentially quite interesting effects in microgravity.

Clark, Noel A.↗

NASA NTRS2000

Structure, Hydrodynamics, and Phase Transition of Freely Suspended Liquid Crystals

Smectic liquid crystals are phases of rod shaped molecules organized into one dimensionally (1D) periodic arrays of layers, each layer being between one and two molecular lengths thick. In the least ordered smectic phases, the smectics A and C, each layer is a two dimensional (2D) liquid. Additionally there are a variety of more ordered smectic phases having hexatic short range translational order or 2D crystalline quasi long range translational order within the layers. The inherent fluid-layer structure and low vapor pressure of smectic liquid crystals enable the long term stabilization of freely suspended, single component, layered fluid films as thin as 30A, a single molecular layer. The layering forces the films to be an integral number of smectic layers thick, quantizing their thickness in layer units and forcing a film of a particular number of layers to be physically homogeneous with respect to its layer structure over its entire area. Optical reflectivity enables the precise determination of the number of layers. These ultrathin freely suspended liquid crystal films are structures of fundamental interest in condensed matter and fluid physics. They are the thinnest known stable condensed phase fluid structures and have the largest surface-to-volume ratio of any stable fluid preparation, making them ideal for the study of the effects of reduced dimensionality on phase behavior and on fluctuation and interface phenomena. Their low vapor pressure and quantized thickness enable the effective use of microgravity to extend the study of basic capillary phenomena to ultrathin fluid films. Freely suspended films have been a wellspring of new liquid crystal physics. They have been used to provide unique experimental conditions for the study of condensed phase transitions in two dimensions. They are the only system in which the hexatic has been unambiguously identified as a phase of matter, and the only physical system in which fluctuations of a 2D XY system and Kosterlitz Thouless phase transition has been observed and 2D XY quasi long range order verified. Smectic films have enabled the precise determination of smectic layer electron density and positional fluctuation profile and have been used to show that the interlayer interactions in anti-ferroelectric tilted smectics do not extend significantly beyond nearest neighbors. The interactions which are operative in liquid crystals are generally weak in comparison to those in crystalline phases, leading to the facile manipulation of the order in liquid crystals by external agents such as applied fields and surfaces. Effects arising from weak ordering are significantly enhanced in ultrathin free films and filaments wherein the intermolecular coupling is effectively reduced by loss of neighbors. Over the past four years this research, which we now detail, has produced a host of exciting new discoveries and unexpected results, maintaining the position of the study of freely suspended liquid crystal structures as one of most exciting and fruitful areas of complex fluid physics. In addition, several potentially interesting microgravity free film experiments have been identified.

Clark, Noel A.↗

NASA NTRS2000

Structural Characterization of Crystalline Ice Nanoclusters

Water ice nanoclusters are useful analogs for studying a variety of processes that occur within icy grains in the extraterrestrial environment. The surface of ice nanoclusters prepared in the laboratory is similar to the surface of interstellar ice grains. In cold molecular clouds, the silicate cores of interstellar grains are typically approx. 100 nm in diameter and have a coating of impure amorphous water ice. Depositional, thermal and radiolytic processes leave the surface and subsurface molecules in a disordered state. In this state, structural defects become mobile and reactions of trapped gases and small molecules can occur. The large surface area of nanocluster deposits relative to their bulk allows for routine observation of such surface-mediated processes. Furthermore, the disordered surface and subsurface layers in nanocluster deposits mimic the structure of amorphous ice rinds found on interstellar dust grains. Transmission Electron Microscopy (TEM has been used tn characterize the crystallinity, growth mechanism, and size distribution of nanoclusters formed from a mixture of water vapor with an inert carrier gas that has been rapidly cooled to 77K. E M imaging reveals a Gaussian size distribution around a modal diameter that increases from approx. 15 to 30 nm as the percentage of water vapor within the mixture increases from 0.5 to 2.007, respectively . TEM bright and dark field imaging also reveals the crystalline nature of the clusters. h4any of the clusters show a mosaic structure in which crystalline domains originate at the center Other images show mirror planes that are separated by approx. 10 nm. Electron diffraction patterns of these clusters show that the clusters are composed of cubic ice with only a small hexagonal component. Further, the crystalline domain size is approximately the same as the modal diameter suggesting that the clusters are single crystals.

Blake, David↗

NASA NTRS1999

Crystal Growth Using MEPHISTO

The shuttle flight experiment "In Situ Monitoring of Crystal Growth Using MEPHISTO" was accomplished during STS-87 as part of the fourth flight of the United States Microgravity Payload (USMP-4), which was flown from November 19 to December 5, 1997. The data returned from that flight are just now beginning to yield quantitative results. This project is an international collaboration: the furnace system known as MEPHISTO was built in France by CNES (French National Space Agency) and CEA (French Atomic Energy Commission); the principal investigator, Prof. Reza Abbaschian, is from the University of Florida at Gainesville; and numerical and analytical modeling support includes collaborators from the University of New South Wales, Australia, the University of Wisconsin at Milwaukee, the National Institute of Standards and Technology, and the NASA Lewis Research Center. MEPHISTO is a French acronym that translates into English as Materials for the Study of Interesting Phenomena of Solidification on Earth and in Orbit. Since this was the fourth flight of the MEPHISTO furnace, the experiment is referred to as MEPHISTO-4. MEPHISTO-4 was a directional solidification experiment that studied the liquid-to-solid transformation of bismuth alloyed with tin. Directional solidification is a freezing technique common to the processing of the electronic materials used in integrated circuits and detectors, such as silicon and germanium. When liquids are frozen on Earth, they must be cooled. The cooling causes stirring because of density variations in the liquid. This stirring, known as natural convection, influences the quality of the resulting solid. During freezing, regions of high and low concentrations of tin are created. This introduces another important phenomenon: diffusion, or the movement by molecular action of matter from regions of high concentration to regions of lower concentration. In MEPHISTO-4, it is tin that diffuses from the high-concentration region in front of the solid-liquid interface to more distant low-concentration regions.

deGroh, Henry C., III↗

NASA NTRS2005

N-Type delta Doping of High-Purity Silicon Imaging Arrays

A process for n-type (electron-donor) delta doping has shown promise as a means of modifying back-illuminated image detectors made from n-doped high-purity silicon to enable them to detect high-energy photons (ultraviolet and x-rays) and low-energy charged particles (electrons and ions). This process is applicable to imaging detectors of several types, including charge-coupled devices, hybrid devices, and complementary metal oxide/semiconductor detector arrays. Delta doping is so named because its density-vs.-depth characteristic is reminiscent of the Dirac delta function (impulse function): the dopant is highly concentrated in a very thin layer. Preferably, the dopant is concentrated in one or at most two atomic layers in a crystal plane and, therefore, delta doping is also known as atomic-plane doping. The use of doping to enable detection of high-energy photons and low-energy particles was reported in several prior NASA Tech Briefs articles. As described in more detail in those articles, the main benefit afforded by delta doping of a back-illuminated silicon detector is to eliminate a "dead" layer at the back surface of the silicon wherein high-energy photons and low-energy particles are absorbed without detection. An additional benefit is that the delta-doped layer can serve as a back-side electrical contact. Delta doping of p-type silicon detectors is well established. The development of the present process addresses concerns specific to the delta doping of high-purity silicon detectors, which are typically n-type. The present process involves relatively low temperatures, is fully compatible with other processes used to fabricate the detectors, and does not entail interruption of those processes. Indeed, this process can be the last stage in the fabrication of an imaging detector that has, in all other respects, already been fully processed, including metallized. This process includes molecular-beam epitaxy (MBE) for deposition of three layers, including metallization. The success of the process depends on accurate temperature control, surface treatment, growth of high-quality crystalline silicon, and precise control of thicknesses of layers. MBE affords the necessary nanometer- scale control of the placement of atoms for delta doping. More specifically, the process consists of MBE deposition of a thin silicon buffer layer, the n-type delta doping layer, and a thin silicon cap layer. The n dopant selected for initial experiments was antimony, but other n dopants as (phosphorus or arsenic) could be used. All n-type dopants in silicon tend to surface-segregate during growth, leading to a broadened dopant-concentration- versus-depth profile. In order to keep the profile as narrow as possible, the substrate temperature is held below 300 C during deposition of the silicon cap layer onto the antimony delta layer. The deposition of silicon includes a silicon- surface-preparation step, involving H-termination, that enables the growth of high-quality crystalline silicon at the relatively low temperature with close to full electrical activation of donors in the surface layer.

Blacksberg, Jordana↗

NASA NTRS1995

The glycan keratan sulfate in inner ear crystals

The otoconial matrix (OM) of chicks (Gallus domesticus) inner ear was analyzed. Histochemically the OM was reacted with phosphotungstic acid (PTA) and immunohistochemically with the monoclonal antibody antikeratan sulfate (antiKS). The OM was digested with the enzyme endo-beta-galactosidase (E beta Galase) or separated by 1D and 2D gel electrophoresis. PTA which reacts with glycoproteins precipitated the OM, suggesting that the OM contains glycoproteins. A central core in each crystal had no PTA staining, suggesting that the core lacked glycoproteins. Anti KS antibody stained the OM with increased density in older embryos as determined by color thresholding. E beta Galase, which cleaves the lactosamine repeating units in KS, decreased the immunostain by 30% in the OM and by 20% in the cartilage. The OM from the utricle, saccule and macula lagena contained similar molecular weight bands. Five dense bands in the OM were less dense in tissue and blood controls, suggesting that such bands are enriched in the OM. Isoelectric focusing of the OM showed a negatively charged high molecular weight smear not present in blood and faint in tissue controls. The high affinity of the OM for the cationic PTA stain, the strong immunohistochemical reaction of the OM with anti KS antibody and high molecular weight negative smear in 2D gels taken together suggest that: a) the OM contains large amounts of glycoproteins and glycans, one of which is keratan sulfate, because its immuno stain with antiKS antibody was decreased by the enzyme E beta Galase, b) the utricle, saccule and macula lagena may have similar composition, and c) the concentration of KS may increase gradually until complete mineralization of the OM is reached.

Non-NASA Center↗

NASA NTRS1995

The statolith compartment in Chara rhizoids contains carbohydrate and protein

In contrast to higher plants, the alga Chara has rhizoids with single membrane-bound compartments that function as statoliths in gravity perception. Previous work has demonstrated that these statoliths contain barium sulfate crystals. In this study, we show that statoliths in Chara rhizoids react with a Coomassie Brilliant Blue cytochemical stain for proteins. While statoliths did not react with silver methenamine carbohydrate cytochemistry, the monoclonal antibody CCRC-M2, which is against a carbohydrate (sycamore-maple rhamnogalacturonan I), labeled the statolith compartment. These results demonstrate that in addition to barium sulfate, statoliths in Chara rhizoids have an organic matrix that consists of protein and carbohydrate moieties. Since the statoliths were silver methenamine negative, the carbohydrate in this compartment could be a 3-linked polysaccharide. CCRC-M2 also labeled Golgi cisternae, Golgi-associated vesicles, apical vesicles, and cell walls in the rhizoids. The specificity of CCRC-M2 immunolabeling was verified by several control experiments, including the demonstration that labeling was abolished when the antibody was preabsorbed with its antigen. Since in this and a previous study (John Z. Kiss and L. Andrew Staehelin, American Journal of Botany 80: 273-282, 1993) antibodies against higher plant carbohydrates crossreacted with cell walls of Chara in a specific manner, Characean algae may be a useful model system in biochemical and molecular studies of cell walls.

NASA Discipline Plant Biology↗