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The materials processing research base of the Materials Processing Center

An annual report of the research activities of the Materials Processing Center of the Massachusetts Institute of Technology is given. Research on dielectrophoresis in the microgravity environment, phase separation kinetics in immiscible liquids, transport properties of droplet clusters in gravity-free fields, probes and monitors for the study of solidification of molten semiconductors, fluid mechanics and mass transfer in melt crystal growth, and heat flow control and segregation in directional solidification are discussed.

Latanision, R. M.↗

Two-color holography concept (T-CHI)

The Material Processing in the Space Program of NASA-MSFC was active in developing numerous optical techniques for the characterization of fluids in the vicinity of various materials during crystallization and/or solidification. Two-color holographic interferometry demonstrates that temperature and concentration separation in transparent (T-CHI) model systems is possible. The experiments were performed for particular (succinonitrile) systems. Several solutions are possible in Microgravity Sciences and Applications (MSA) experiments on future Shuttle missions. The theory of the T-CHI concept is evaluated. Although particular cases are used for explanations, the concepts developed will be universal. A breadboard system design is also presented for ultimate fabrication and testing of theoretical findings. New developments in holography involving optical fibers and diode lasers are also incorporated.

Vikram, C. S.↗

Effects of microgravity on urinary osteopontin

Increased risk of renal stone formation during space flight has been linked primarily to increased calcium excretion from bone demineralization induced by space flight. Other factors contributing to increased risk include increased urinary calcium oxalate supersaturation, while urinary citrate, magnesium and volume are all decreased. The aim of this study was to increase the predictive value of stone risk profiles for crew members during space flight by evaluating the excretion of urinary protein inhibitors of calcium crystallization so that more comprehensive stone risk profiles could relate mineral saturation to the concentrations of inhibitor proteins. Levels of urinary osteopontin (uropontin) are reported in a series of 14 astronauts studied before, during, and after space flights. During space flight, a compensatory increase in uropontin excretion was not observed. However, the uropontin excretion of a majority of astronauts was increased during the period after space flight and was maximal at 2 wk after landing. The downward shift in the molecular size of uropontin observed in samples obtained during space flight was shown to result from storage at ambient temperature during flight, rather than an effect of microgravity on uropontin synthesis.

NASA Experiment Number 9401651↗

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.↗

Experimental correlation of melt structures, nucleation rates, and thermal histories of silicate melts

The theory and measurement of the structure of liquids is an important aspect of modern metallurgy and igneous petrology. Liquid structure exerts strong controls on both the types of crystals that may precipitate from melts and on the chemical composition of those crystals. An interesting aspect of melt structure studies is the problem of melt memories; that is, a melt can retain a memory of previous thermal history. This memory can influence both nucleation behavior and crystal composition. This melt memory may be characterized quantitatively with techniques such as Raman, infrared and NMR spectroscopy to provide information on short-range structure. Melt structure studies at high temperature will take advantage of the microgravity conditions of the Space Station to perform containerless experiments. Melt structure determinations at high temperature (experiments that are greatly facilitated by containerless technology) will provide invaluable information for materials science, glass technology, and geochemistry. In conjunction with studies of nucleation behavior and nucleation rates, information relevant to nucleation in magma chambers in terrestrial planets will be acquired.

Boynton, W. V.↗

Polymer morphologh

All polymeric materials in their final application are aggregates of many molecules. For linear macromolecules, these aggregates are highly entangled and their macroscopic properties are affected in a little-known way by the interpenetration and entanglements of the molecules. Over the years, we have done occasional investigations of single molecule single crystals and found that there are many unsolved questions about their nucleation, growth, kinetically determined shape, and ultimate path to equilibrium morphology on annealing. This initial work could be extended by a study of the applicability of microgravity methods for the production and study of the formation of single molecule particles. The production of separated molecules of sufficient size to produce phase-like behavior would involve perhaps a spray of solutions containing single molecules, followed by evaporation of the volatiles, or precipitation out of dispersion droplets. Other methods may involve Langmuir films etc., as shown in our prior work. The microgravity environment should enhance the efficiency of any of these methods by avoiding the joining of growing particles by reduction of convection and settling due to density differences. Once produced, the single molecule droplets are to be quenched into the glassy state and analyzed morphologically and thermally. Their shape alone can be used for molecular mass determination (an old problem that suffered from the need to estimate the shape of collapsed (flat) droplets on a surface). Next would be the study of changes of properties as a function of time, temperature, and molecular mass (and distribution) on fusion to macroscopic single phases.

Wunderlich, Bernhard↗

Dendritic solidification under microgravity conditions

The Isothermal Dendritic Growth Experiment is undergoing development in cooperation with NASA-Lewis in order to test dendritic growth theory at small supercoolings in low earth orbit. The apparatus encompasses four major subsystems: a temperature-controlled thermostatic bath capable of millikelvin stability, a photographic data collection system, a crystal-growth chamber, and a start-detection system which initiates data collection. Comparisons are made with ground-based study methods for dendritic growth.

Glicksman, M. E.↗

Draft Genome Sequences of Biosafety Level 2 Opportunistic Pathogens Isolated From the Environmental Surfaces of the International Space Station

The draft genome sequences of 20 biosafety level 2 (BSL-2) opportunistic pathogens isolated from the environmental surfaces of the International Space Station (ISS) were presented. These genomic sequences will help in understanding the influence of microgravity on the pathogenicity and virulence of these strains when compared with Earth strains.

Aleksandra Checinska Sielaff↗

Reverse Micelle Based Synthesis of Microporous Materials in Microgravity

Microporous materials include a large group of solids of varying chemical composition as well as porosity. These materials are characterized by channels and cavities of molecular dimensions. The framework structure is made up of interconnecting T-O-T' bonds, where T and T' can be Si, Al, P, Ga, Fe, Co, Zn, B and a host of other elements. Materials with Si-O-Al bonding in the framework are called zeolites and are extensively used in many applications. Ion-exchange properties of these materials are exploited in the consumer and environmental industries. Chemical and petroleum industries use zeolites as catalysts in hydrocarbon transform ations. Synthesis of new microporous frameworks has led to the development of new technologies, and thus considerable effort worldwide is expended in their discovery. Microporous materials are typically made under hydrothermal conditions. Influence of nature of starting reactants, structure directing agents, pH, temperature, and aging all have profound influence on the synthesis process. This is primarily because the most interesting open frameworks are not necessarily the stable structures in the reaction medium. Thus, the discovery of new frameworks is often tied to finding the right composition and synthesis conditions that allow for kinetic stabilization of the structure. This complexity of the synthesis process and limited understanding of it has made it difficult to develop directed is of microporous materials and most advances in this field have been made by trial and error. The basic issues in crystal growth of these materials include: (1) Nature of the nucleation process; (2) Molecular structure and assembly of nuclei; (3) Growth of nuclei into crystals; (4) Morphology control; and (5) Transformation of frameworks into other structures. The NASA-funded research described in this paper focuses on all the above issues and has been described in several publications. We present the highlights of our program, especially with the focus on possible experiments in microgravity.

Dutta, Prabir K.↗

Space Product Development of Commercial NLO Materials

Growth on selected substrates under various processing conditions have been useful for preparing highly oriented and otherwise promising films of organic compounds for optical thin films and waveguides. The significance of processing conditions to uniformity in thickness, degree of orientation, film quality, and optical properties for a specific processing technique is the general focus of work in this area. A study on the effect of processing conditions relevant to thin-film deposition by various techniques is particularly difficult because of the possibility that convection may play a major role in some cases. It is a goal of some researchers to produce good quality anisotropic films, therefore, an important, yet understudied, requirement should be to assess the role of gravity during certain processing methods. This may be particularly true for the vapor deposition of diacetylenes where subsequent polymerization in the crystal is topochemical and occurs readily only when neighboring monomer molecules are sufficiently close and suitably oriented. Likewise, this requirement is equally viable for the vapor deposition of certain materials such as Pcs in view of the results of microgravity experiments by 3M Corporation involving the preparation of thin films of copper Pc (CuPc). Microgravity-grown CuPc had several desirable features which indicate that the vapor growth of organic films in low-g may result in better quality films for optical and electrical applications. Indeed, other materials vapor deposited onto specific substrates in microgravity produce films potentially beneficial for electro-optic applications. A novel technique, recently discovered, for growing polydiacetylene thin films involves exposing a transparent substrate, in contact with diacetylene monomer solution, to ultraviolet (LTV) light. A polymer film deposits on the side of the substrate in contact with monomer in solution, and there are distinct gravitational effects, which influence film quality. Good quality thin films elude growth from solutions absent of uniform flow fields and homogeneous temperature distributions near the substrate surfaces. The flow fields and temperature distributions during the polymerization process by exposure to UV light details the nature of gravitational influences on this process.

Frazier, Donald O.↗

SAMS Acceleration Measurements on Mir from November 1995 to March 1996

The NASA Microgravity Science and Applications Division (MSAD) sponsors science experiments on a variety of microgravity carriers, including Orbiter missions and Russia's Mir space station. The MSAD sponsors the Space Acceleration Measurement System (SAMS) at the NASA Lewis Research Center (LERC) to support these science experiments by providing acceleration measurements to characterize the microgravity environment to which the experiments were exposed. The LeRC Principal Investigator Microgravity Services (PIMS) project supports principal investigations of microgravity science experiments as they evaluate the effects of varying acceleration levels on their experiments. In 1994, a SAMS unit was installed on the Mir space station. In a manner similar to Orbiter mission support, the SAMS unit supports science experiments from the U.S. and Russia by measuring the microgravity environment during experiment operations. Previous reports have summarized the SAMS data acquired during the period from September 1994 to November 1995. During the time period from November 1995 to March 1996, the primary SAMS-supported experiment was a Protein Crystal Growth (PCG) experiment. SAMS data were obtained during the PCG operations on Mir in accordance with the requirements specified by the PCG Principal Investigator. Also included in this data are mission events of interest, such as the undocking of STS-74 from Mir (November 1995) and the docking of Atlantis (STS-76) to Mir in March 1996. This report presents an overview of the SAMS data recorded in the interval from November 1995 to March 1996.

DeLombard, Richard↗

Mechanisms for the Crystallization of ZBLAN

A number of research teams have observed that glass forming melts that are solidified in low-g exhibit enhanced glass formation. This project will examine one of these glasses, the heavy metal fluoride glass ZBLAN. A four year ground based research program has been approved to examine the crystallization of ZBLAN glasses with the purpose of testing a theory for the crystallization of ZBLAN glass. The theory could explain the general observations of enhanced glass formation of other glasses melted and solidified in low-g. Fluid flow in 1-g results from buoyancy forces and surface tension driven convection. This fluid flow can introduce shear in undercooled liquids in 1-g. In low-g it is known that fluid flows are greatly reduced so that the shear rate in fluids in low-g are extremely low. It is believed that fluids may have some weak structure in the absence of flow. Even very small shear rates could cause this structure to collapse in response to the shear. A general result would be shear thinning of the fluid. The hypothesis of this research is that: Shear thinning in undercooled liquids increases the rate of nucleation and crystallization of glass forming melts. Shear of the melt can be reduced in low-g enhancing undercooling and glass formation. Samples will be melted and quenched in 1-g under quiescent conditions at a number of controlled cooling rates to determine times and temperatures of crystallization and heated at controlled heating rates to determine kinetic crystallization parameters. Experiments will also be performed on the materials while under controlled vibration conditions and compared with the quiescent experiments in order to evaluate the effect of shear in the liquid on crystallization kinetics. After the experimental parameters are well known, experiments will be repeated under low-g (and 2-g) conditions on the KC-135 aircraft during low-g parabolic maneuvers. The results will determine the effects of shear on crystallization. Our experimental setups will be designed with low-g experiments in mind and will be tested as breadboard low-g experiments. It is very likely that the thermal analysis instrumentation can be adapted to be run in the microgravity glovebox facilities. Critical space experiments may result to test the theory at longer low-g time experiments in space.

Ethridge, Edwin C.↗

Extraordinary Accomplishments of the In Space Production Applications Portfolio in 2024

The purpose of the NASA In-Space Production Applications (InSPA) program is to provide funding and expertise to help brilliant United States innovators and businesses traverse the technology “Valley of Death” by proving out their concepts for in-space manufactured materials and products that will ultimately be sold to customers on the Earth. Scientific and technological advances on the International Space Station (ISS) and on Earth coupled with evolving societal needs are collectively enabling InSPA-funded teams to produce data streams and advanced biological, chemical, and physical materials solutions with economic value. We report on an extraordinary year of accomplishments on the ISS and highlight top InSPA and ISS National Lab results that span historic firsts in cancer research, stem cells, crystal production, optical fiber production, drug discovery, in-space treatments with RNA therapeutics, and production of artificial retinas from space. We assert that the results have enormous potential, are transforming the space exploration ecosystem and are the “seeds” of a microgravity industrial revolution that are shaping national microgravity strategy.

in spa↗

Materials processing in space - Review of the early experiments

Basic research performed to study various aspects of fluid behavior in a microgravity environment during the first two decades of spaceflight is described. The uniqueness of space was recognized in the 1950s as a place where buoyancy-driven convective flows and sedimentation would effectively be absent. The conditions were favorable for experiments in crystal growth, alloy solidification, combustion, thermocapillary flows, electroosmotic flows, Stefan flows, Soret diffusion, and solidification processes. Pre-Skylab NASA drop tower experiments and Apollo 14 and 17 experiments made in preparation for Skylab are described. Skylab welding and brazing, crystal growth, metallurgy and liquid float zone trials and Apollo-Soyuz crystal growth, electrophoresis and metallurgical experiments are summarized. SPAR rocket trials along similar lines are also outlined.

Naumann, Robert J.↗

Isothermal dendritic growth - A proposed microgravity experiment

This paper describes an isothermal dendritic growth experiment (IDGE), a microgravity-oriented spaceborne scientific experiment designed to obtain 'convection-free' dendritic growth and thereby provide a test of dendritic growth theory. The apparatus includes a controlled thermostatic bath capable of providing + or - 2 mK stability, a photographic data collection system, a crystal growth chamber ensuring 'free' dendritic growth, and an optical RAM camera for crystal growth detection. The experiment will be carried on essentially automatically aboard the Materials Science Laboratory in the cargo bay of the Space Shuttle. The results of preliminary ground-based studies are presented.

Glicksman, M. E.↗

Second United States Microgravity Payload: One Year Report

The second United States Microgravity Payload (USMP-2), flown in March 1994, carried four major microgravity experiments plus a sophisticated accelerometer system. The USMP program is designed to accommodate experiments requiring extensive resources short of a full Spacelab mission. The four USMP-2 experiments dealt with understanding fundamental aspects of materials behavior, three with the formation of crystals from melts and one with the critical point of a noble gas. This successful, scientifically rich mission also demonstrated telescience operations.

Curreri, Peter A.↗

Detached Growth of Germanium and Germaniumsilicon

Up to now, detached growth was observed mainly under microgravity, i.e. under the absence of hydrostatic pressure that hinders the formation of a free melt meniscus. the detached growth of germanium doped with gallium was obtained under 1 g conditions, the growth was performed in quartz-glass ampoule. Part of the crystal grew without wall contact, the detached growth was observed in-situ with a CCD-camera as well as after the growth process in form of growth lines and the formation of <111> facets on the crystal surface. GeSi crystal (oriientation: <111>, maximum silicon content: 4 at%, seed material: Ge) was grown in a pBN crucible (excluding the possibility of in-situ monitoring of the growth process). The grown crystal exhibits three growth facets, indicating also wall free growth. Surface analysis of the crystals (NDIC, SEM) and characterization of crystal segregation (EDAX, resistivity measurement) and defect structure (EPD, x-ray diffraction measurements) will be presented.

Dold, P.↗

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.↗