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Continuous Czochralski growth. Development of advanced Czochralski growth process to produce low cost 150 kg silicon ingots from a single crucible for technology readiness

The improvement of growth rates using radiation shielding and investigation of the crucible melt interaction for improved yields were emphasized. Growth runs were performed from both 15 and 16 inch diameter crucibles, producing 30 and 37 kg ingots respectively. Efforts to increase the growth rate of 150 mm diameter ingots were limited by temperature instabilities believed to be caused by undesirable thermal convections in the larger melts. The radiation shield improved the growth rate somewhat, but the thermal instability was still evident, leading to nonround ingots and loss of dislocation-free structure. A 38 kg crystal was grown to demonstrate the feasibility of producing 150 kg with four growth cycles. After the grower construction phase, the Hamco microprocessor control system was interfaced to the growth facility, including the sensor for automatic control of seeding temperature, and the sensor for automatic shouldering. Efforts focused upon optimization of the seeding, necking, and shoulder growth automation programs.

Source record↗

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↗

Growth of CdZnTe Crystals the Bridgman Technique with Controlled Overpressures of Cd

Cd(1-x)Zn(x)Te crystals with x = 0.15 and 0.20, were grown in this study by closed-ampoule directional solidification (Bridgman) technique with a controlled Cd overpressure. The growth ampoule was made of quartz with inner diameter from 20 to 40 mm and a tapered length of 2.5 cm at the growth tip. Both unseeded and seeded growths were performed with total material charges up to 400 g. After the loading of starting CdZnTe material, a typical amount of 2 g of Cd was also loaded inside a Cd reservoir basket, which was attached beneath the seal-off cup. The ampoule was sealed off under a vacuum below lxl0(exp -5) Torr. The sealed ampoule was placed inside a 4-zone Bridgman furnace - a Cd reservoir zone with a heat-pipe furnace liner on the top, followed by a hot zone, a booster heating zone and a cold zone at the bottom. The Cd zone was typically 300 to 400 C below the hot zone setting. High resistivity material has been obtained without any intentional dopants but has been reproducibly obtained with In doping. The crystalline and the electrical properties of the crystals will be reported.

Su, Ching-Hu↗

A New Look at the Environmental Conditions Favorable to Secondary Ice Production

This study attempts a new identification of mechanisms of secondary ice production (SIP) based on the observation of small faceted ice crystals (hexagonal plates or columns) with typical sizes smaller than 100µm. Due to their young age, such small ice crystals can be used as tracers for identifying the conditions for SIP. Observations reported here were conducted in oceanic tropical mesoscale convective systems (MCSs) and midlatitude frontal clouds in the temperature range from 0 to −15◦C and heavily seeded by aged ice particles. It was found that in both MCSs and frontal clouds, SIP was observed right above the melting layer and extended to higher altitudes with colder temperatures. The roles of six possible mechanisms to generate the SIP particles are assessed using additional observations. In most observed SIP cases, small secondary ice particles spatially correlated with liquid-phase, vertical updrafts and aged rimed ice particles. However, in many cases, neither graupel nor liquid drops were observed in the SIP regions, and therefore, the conditions for an active Hallett–Mossop process were not met. In many cases, large concentrations of small pristine ice particles were observed right above the melting layer, starting at temperatures as warm as −0.5◦C. It is proposed that the initiation of SIP above the melting layer is stimulated by the recirculation of large liquid drops through the melting layer with convective turbulent updrafts. After re-entering a super cooled environment above the melting layer, they impact with aged ice, freeze, and shatter. The size of the splinters generated during SIP was estimated as 10µm or less. A principal conclusion of this work is that only the freezing drop-shattering mechanism could be clearly supported by the airborne in situ observations.

Korolev, Alexei↗

Microencapsulation of anti-tumor, antibiotic and thrombolytic drugs in microgravity

Encapsulation of cytotoxic or labile drugs enables targeted delivery and sustained release kinetics that are not available with intravenous injection. A new liquid-liquid diffusion process has been developed for forming unique microcapsules that contain both aqueous and hydrocarbon soluble drugs. Microgravity experiments, on sounding rockets (1989-92) and Shuttle missions STS-52 (1992) and STS-56 (1993) using an automated Materials Dispersion Apparatus, produced multi-lamellar microcapsules containing both Cis-platinum (anti-tumor drug) and iodinated poppy seed oil (a radiocontrast medium), surrounded by a polyglyceride skin. Microcapsules formed with amoxicillin (antibiotic) or urokinase (a clot dissolving enzyme), co-encapsulated with IPO, are still intact after two years. Microcapsules were formed with the drug so concentrated that crystals formed inside. Multi-layered microspheres, with both hydrophobic drug compartments, can enable diffusion of complementary drugs from the same microcapsule, e.g. antibiotics and immuno-stimulants to treat resistant infections or multiple fibrinolytic drugs to dissolve emboli. Co-encapsulation of enough radio-contrast medium enables oncologists to monitor the delivery of anti-tumor microcapsules to target tumors using computerized tomography and radiography that would track the distribution of microcapsules after release from the intra-arterial catheter. These microcapsules could have important applications in chemotheraphy of certain liver, kidney, brain and other tumors.

Morrison, Dennis R.↗

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↗

Phase transformations in ion-irradiated silicides

The present investigation has three objectives. The first is concerned with the phase transformation of CoSi2 under ion implantation and the subsequent crystallization characteristics during annealing, taking into account epitaxial and nonepitaxial recrystallization behavior. The second objective is related to a study of the general trend of implantation-induced damage and crystallization behavior for a number of commonly used silicides. The last objective involves a comparison of the recrystallization behavior of cosputtered refractory silicides with that of the ion-implanted silicides. It was found that epitaxial regrowth of ion-irradiated CoSi2 occurred for samples with an epitaxial seed left at the Si/CoSi2 interface. A structural investigation of CoSi2 involving transmission electron microscopy (TEM) showed that after high-dose implantation CoSi2 is amorphous.

Hewett, C. A.↗

Growth of Solid Solution Single Crystals

The solidification of a solid solution semiconductor, having a wide separation between liquidus and serious has been extensively studied in ground based, high magnetic field and Spacelab experiments. Two alloys of mercury cadmium telluride have been studied; mercury cadmium telluride with 80.0 mole percent of HgTe and 84.8 mole percent respectively. These alloys are extremely difficult to grow by directional solidification on earth due to high solutal and thermal density differences that give rise to fluid flow and consequent loss of interface shape and composition. Diffusion controlled growth is therefore impossible to achieve in conventional directional solidification. The ground based experiments consisted of growing crystals in several different configurations of heat pipe furnaces, NASA's Advanced Automated Directional Solidification Furnace (AADSF), and a similar furnace incorporated in a superconducting magnet capable of operating at up to 5T. The first microgravity experiment took place during the flight of STS-62 in March 1994, with the AADSF installed on the second United States Microgravity Payload (USMP-2). The alloy was solidified at 3/4 inch per day over a 9 day period, and for the first time a detailed evaluation was performed of residual acceleration effects. The second flight experiment took place in the fourth United States Microgravity Payload Mission (USMP-4) in November 1997. Due to contamination of the furnace system by a previously processed sample, the sample was not received until May 1998, and the preliminary analysis shows that the conditions prevailing during the experiment were quite different from the requirements requested prior to the mission. Early results are indicating that the sample may not accomplish the desired objectives. As with the USMP-2 mission, the results of the ground based experiments were compared with the crystal grown in orbit under microgravity conditions. On the earth, it has been demonstrated that the application of the magnetic field leads to a significant reduction in fluid flow, with improved homogeneity of composition. The field strength required to suppress flow increases with diameter of the material. The 8 mm diameter sample used here was less than the upper diameter limit for a ST magnet. The configuration for USMP-4 was changed so that the material was seeded and other processing techniques were also modified. It was decided to examine the effects of a strong magnetic field under the modified configuration and parameters. A further change from USMP-2 was that a different composition of material was grown, namely with 0.152 mole fraction of cadmium telluride rather than the 0.200 of the USMP-2 experiment. The objective was to grow highly homogeneous, low defect density material of a composition at which the conduction band and the valence band of the material impinge against each other. As indicated, the furnace was contaminated during the mission. As a result of solid debris remaining in the furnace bore, the cartridge in this experiment, denoted as SL1-417, was significantly bent during the insertion phase. During translation the cartridge scraped against the plate which isolates the hot and cold zones of the furnace. Thermocouples indicated that a thermal assymetry resulted. The scraping in the slow translation or crystal growth part of the processing was not smooth and it is probable that the jitter was sufficient to give rise to convection in the melt. Early measurements of composition from the surface of the sample have shown that the composition varies in an oscillatory manner.

Lehoczky, Sandor L.↗

A Hybrid Fiber/Solid-State Regenerative Amplifier with Tunable Pulse Widths for Satellite Laser Ranging

A fiber/solid-state hybrid seeded regenerative amplifier, capable of achieving high output energy with tunable pulse widths, has been developed for satellite laser ranging applications. The regenerative amplifier cavity uses a pair of Nd:YAG zigzag slabs oriented orthogonally to one another in order to make thermal lensing effects symmetrical and simplify optical correction schemes. The seed laser used is a fiber-coupled 1,064-nm narrowband (<0.02 nm) diode laser that is discretely driven in a new short-pulsed mode, enabling continuously tunable seed pulse widths in the 0.2-to-0.4-ns range. The amplifier gain unit consists of a pair of Brewster-cut 6-bounce zigzag Nd:YAG laser slabs, oriented 90deg relative to each other in the amplifier head. This arrangement creates a net-symmetrical thermal lens effect (an opposing singleaxis effect in each slab), and makes thermo-optical corrections simple by optimizing the curvature of the nearest cavity mirror. Each slab is pumped by a single 120-W, pulsed 808-nm laser diode array. In this configuration, the average pump beam distribution in the slabs had a 1-D Gaussian shape, which matches the estimated cavity mode size. A half-wave plate between the slabs reduces losses from Fresnel reflections due to the orthogonal slabs Brewster-cut end faces. Successful "temporal" seeding of the regenerative amplifier cavity results in a cavity Q-switch pulse envelope segmenting into shorter pulses, each having the width of the input seed, and having a uniform temporal separation corresponding to the cavity round-trip time of approx. =10 ns. The pulse energy is allowed to build on successive passes in the regenerative amplifier cavity until a maximum is reached, (when cavity gains and losses are equal), after which the pulse is electro- optically switched out on the next round trip The overall gain of the amplifier is approx. =82 dB (or a factor of 1.26 million). After directing the amplified output through a LBO frequency doubling crystal, approx. = 2.1 W of 532-nm output (>1 mJ) was measured. This corresponds to a nonlinear conversion efficiency of >60%. Furthermore, by pulse pumping this system, a single pulse per laser shot can be created for the SLR (satellite laser ranging) measurement, and this can be ejected into the instrument. This is operated at the precise frequency needed by the measurement, as opposed to commercial short-pulsed, mode-locked systems that need to operate in a continuous fashion, or CW (continuous wave), and create pulses at many MHz. Therefore, this design does not need to throw away or dump 99% of the laser energy to produce what is required; this system can be far smaller, more efficient, cheaper, and readily deployed in the field when packaged efficiently. Finally, by producing custom diode seed pulses electronically, two major advantages over commercial systems are realized: First, this pulse shape is customizable and not affected by the cavity length or gain of the amplifier cavity, and second, it can produce adjustable (selectable) pulse widths by simply adding multiple seed diodes and coupling each into commercial, low-cost fiber-optic combiners.

Coyle, Barry↗

Directional Solidification of Mercury Cadmium Telluride in Microgravity

Mercury cadmium telluride (MCT) has been directionally solidified for ten days in the Advanced Automated Directional Solidification Furnace (AADSF) on the second United States Microgravity Payload Mission (USMP-2). A second growth experiment is planned for the USMP-4 mission in November 1997. Results from USMP-2 demonstrated significant changes between microgravity and ground-based experiments, particularly in the compositional homogeneity. Changes were also observed during the microgravity mission which were dependent on the attitude of the space shuttle and the relative magnitudes of axial and transverse residual accelerations with respect to the growth axis of the crystal. Issues of shuttle operation, especially those concerned with safety and navigation, and the science needs of other payloads dictated the need for changes in attitude. One consequence for solidification of MCT in the USMP4 mission is the desire for a shorter growth time to complete the experiment without subjecting the sample to shuttle maneuvers. By using a seeded technique and a pre-processed boule of MCT with an established diffusion layer quenched into the solid, equilibrium steady state growth can be established within 24 hours, rather than the three days needed in USMP-2. The growth of MCT in AADSF during the USMP-4 mission has been planned to take less than 72 hours with 48 hours of actual growth time. A review of the USMP-2 results will be presented, and the rationale for the USMP-4 explained. Pre-mission ground based tests for the USN4P-4 mission will be presented, as will any available preliminary flight results from the mission.

Lechoczhy, Sandor L.↗

Optical diagnostics of solution crystal growth

Solution crystal growth monitoring of LAP/TGS crystals by various optical diagnostics systems, such as conventional and Mach-Zehnder (M-Z) interferometers, optical heterodyne technique, and ellipsometry, is under development. The study of the dynamics of the crystal growth process requires a detailed knowledge of crystal growth rate and the concentration gradient near growing crystals in aqueous solution. Crystal growth rate can be measured using conventional interferometry. Laser beam reflections from the crystal front as well as the back surface interfere with each other, and the fringe shift due to the growing crystal yields information about the growth rate. Our preliminary results indicate a growth rate of 6 A/sec for LAP crystals grown from solution. Single wavelength M-Z interferometry is in use to calculate the concentration gradient near the crystal. Preliminary investigation is in progress using an M-Z interferometer with 2 cm beam diameter to cover the front region of the growing crystal. In the optical heterodyne technique, phase difference between two rf signals (250 KHZ) is measured of which one is a reference signal, and the other growth signal, whose phase changes due to a change in path length as the material grows. From the phase difference the growth rate can also be calculated. Our preliminary results indicate a growth rate of 1.5 A/sec. the seed and solution temperatures were 26.46 C and 27.92 C respectively, and the solution was saturated at 29.0 C. an ellipsometer to measure the growth rate and interface layer is on order from JOBIN YVON, France. All these systems are arranged in such a manner that measurements can be made either sequentially or simultaneously. These techniques will be adapted for flight experiment.

Kim, Yongkee↗

Lateral Growth Expansion of 4H/6H-SiC m-plane Pseudo Fiber Crystals by Hot Wall CVD Epitaxy

Lateral expansion of small mixed polytype 4H/6H-SiC slivers were realized by hot wall chemical vapor deposition (HWCVD). Small slivers cut from m-oriented ..11..00.. SiC boule slices containing regions of 4H and 6H SiC were exposed to HWCVD conditions using standard silane/propane chemistry for a period of up to eight hours. The slivers exhibited approximately 1500 microns (1.5 mm) of total lateral expansion. Initial analysis by synchrotron white beam x-ray topography (SWBXT) confirms, that the lateral growth was homoepitaxial, matching the polytype of the respective underlying region of the seed sliver.

Trunek, Andrew J.↗

Boundary Layer Measurements in a Supersonic Wind Tunnel Using Doppler Global Velocimetry

A modified Doppler Global Velocimeter (DGV) was developed to measure the velocity within the boundary layer above a flat plate in a supersonic flow. Classic laser velocimetry (LV) approaches could not be used since the model surface was composed of a glass-ceramic insulator in support of heat-transfer measurements. Since surface flare limited the use of external LV techniques and windows placed in the model would change the heat transfer characteristics of the flat plate, a novel approach was developed. The input laser beam was divided into nine equal power beams and each transmitted through optical fibers to a small cavity within the model. The beams were then directed through 1.6-mm diameter orifices to form a series of orthogonal beams emitted from the model and aligned with the tunnel centerline to approximate a laser light sheet. Scattered light from 0.1-micron diameter water condensation ice crystals was collected by four 5-mm diameter lenses and transmitted by their respective optical fiber bundles to terminate at the image plane of a standard two-camera DGV receiver. Flow measurements were made over a range from 0.5-mm above the surface to the freestream at Mach 3.51 in steady state and heat pulse injected flows. This technique provides a unique option for measuring boundary layers in supersonic flows where seeding the flow is problematic or where the experimental apparatus does not provide the optical access required by other techniques.

Meyers, James F.↗

Temperature conditions for chondrule formation

An attempt is made to constrain the chondrule-forming process from dynamic crystallization experiments on chondrule analogs and from correlations between texture and bulk composition in natural chondrules. Liquidus temperatures for chondrules from unequilibrated chondrites are calculated using Herzberg's (1979) method. The paper then infers whether each chondrule formed above, at, or below its liquidus based on textures produced in experiments. A range of temperatures to which chondrules may have been initially heated is then derived from the texture-composition-temperature relationships. Finally, the role of dust seeding, or external heterogeneous nucleation, in producing chondrule textures is examined.

Hewins, Roger H.↗

Ground and Airborne Methane Measurements using Optical Parametric Amplifiers

We report on an initial airborne demonstration of atmospheric methane column measurements at 1.65 micrometers using a widely tunable, seeded optical parametric amplifier (OPA) lidar and a photon counting detector. Methane is an important greenhouse gas and accurate knowledge of its sources and sinks is needed for climate modeling. Our lidar system uses 20 pulses at increasing wavelengths and integrated path differential absorption (IPDA) to map a methane line at 1650.9 nanometers. The wavelengths are generated by using a Nd:YAG pump laser at 1064.5 nanometers and distributed feedback diode laser at 1650.9 nanometers and a periodically-poled lithium niobate (PPLN) crystal. The pulse width was 3 nanoseconds and the pulse repetition rate was 6.28 KHz. The outgoing energy was approximately 13 microJoules/pulse. A commercial 20 nanometer diameter fiber-coupled telescope with a photon counting detector operated in analog mode with a 0.8 nanometer bandpass filter was used as the lidar receiver. The lidar system was integrated on NASA's DC-8 flying laboratory, based at Dryden Airborne operations Facility (DAOF) in Palmdale CA. Three flights were performed in the central valley of California. Each flight lasted about 2.5 hours and it consisted of several flight segments at constant altitudes at approximately 3, 4.5, 6, 7.6, 9.1, 10.6 km (l0, 15, 20, 25, 30, 35 kft). An in-situ cavity ring down spectrometer made by Picarro Inc. was flown along with the lidar instrument provided us with the "truth" i.e. the local CH4, CO2 and H2O concentrations at the constant flight altitude segments. Using the aircraft's altitude, GPS, and meteorological data we calculated the theoretical differential optical depth of the methane absorption at increasing altitudes. Our results showed good agreement between the experimentally derived optical depth measurements from the lidar instrument and theoretical calculations as the flight altitude was increased from 3 to 10.6 kilometers, assuming a constant methane mixing ratio of 1.8 parts per million. The in-situ spectrometer did not show any significant deviations from the ambient concentrations. Further analysis using meteorological data from the Global Modeling and Assimilation Office (http://gmao.gsfc.nasa.gov/) to derive the theoretical optical depth also showed good agreement with the experimentally derived values. The OPA lidar system with slight modifications has also been used to measure CO2, water vapor, and CO in the near and mid-infrared spectral regions on the ground.

Riris, Haris↗

A Compact Ti:Sapphire Laser With its Third Harmonic Generation (THG) for an Airborne Ozone Differential Absorption Lidar (DIAL) Transmitter

A compact and high-pulse-energy Ti:Sapphire laser with its Third Harmonic Generation (THG) has been developed for an airborne ozone differential absorption lidar (DIAL) to study the distributions and concentrations of the ozone throughout the troposphere. The Ti:Sapphire laser, pumped by a frequency-doubled Nd:YAG laser and seeded by a single mode diode laser, is operated either at 867 nm or at 900 nm with a pulse repetition frequency of 20 Hz. High energy laser pulses (more than 110 mJ/pulse) at 867 nm or 900 nm with a desired beam quality have been achieved and utilized to generate its third harmonic at 289nm or 300nm, which are on-line and off-line wavelengths of an airborne ozone DIAL. After being experimentally compared with Beta-Barium Borate (beta - BaB2O4 or BBO) nonlinear crystals, two Lithium Triborate (LBO) crystals (5 x 5 x 20 cu mm) are selected for the Third Harmonic Generation (THG). In this paper, we report the Ti:Sapphire laser at 900 nm and its third harmonic at 300 nm. The desired high ultraviolet (UV) output pulse energy is more than 30 mJ at 300 nm and the energy conversion efficiency from 900 nm to 300 nm is 30%.

Chen, Songsheng↗

Automatic Jet Contrail Detection and Segmentation

Jet contrails are an important subset of cirrus clouds in the atmosphere, and thin cirrus are thought to enhance the greenhouse effect due to their semi-transparent nature. They are nearly transparent to the solar energy reaching the surface, but they reduce the planetary emission to space due to their cold ambient temperatures. Having 'seeded' the environment, contrails often elongate and widen into cirrus-like features. However, there is great uncertainty regarding the impact of contrails on surface temperature and precipitation. With increasing numbers of subsonic aircraft operating in the upper troposphere, there is the possibility of increasing cloudiness which could lead to changes in the radiation balance. Automatic detection and seg- mentation of jet contrails in satellite imagery is important because (1) it is impractical to compile a contrail climatology by hand, and (2) with the segmented images it will be possible to retrieve contrail physical properties such as optical thickness, effective ice crystal diameter and emissivity.

Weiss, J.↗

A modified pump laser system to pump the titanium sapphire laser

As a result of the wide tunability of the titanium sapphire laser NASA has sited it to be used to perform differential absorption lidar (DIAL) measurements of H2O vapor in the upper and lower troposphere. The titanium sapphire laser can provide a spectrally narrow (0.3 to 1.0 pm), high energy (0.5 to 1.0 J) output at 727, 762, and 940 nm which are needed in the DIAL experiments. This laser performance can be obtained by addressing the line-narrowing issues in a master oscillator and the high energy requirement in a fundamental mode oscillator. By injection seeding, the single frequency property of the master oscillator can produce a line narrow high energy power oscillator. A breadboard model of the titanium sapphire laser that will ultimately be used in NASA lidar atmospheric sensing experiment is being designed. The task was to identify and solve any problem that would arise in the actual laser system. One such problem was encountered in the pump laser system. The pump laser that is designed to pump both the master oscillator and power oscillator is a Nd:YLF laser. Nd:YLF exhibits a number of properties which renders this material an attractive option to be used in the laser system. The Nd:YLF crystal is effectively athermal; it produces essentially no thermal lensing and thermally induced birefringence is generally insignificant in comparison to the material birefringence resulting from the uniaxial crystal structure. However, in application repeated fracturing of these laser rods was experience. Because Nd:YLF rods are not commercially available at the sizes needed for this application a modified pump laser system to replace the Nd:YLF laser rod was designed to include the more durable Nd:YAG laser rods. In this design, compensation for the thermal lensing effect that is introduced because of the Nd:YAG laser rods is included.

Petway, Larry B.↗