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All sourcesNASA NTRSDOE OSTI
NASA NTRS2016

An Efficient Single Frequency Ho:YLF Laser for IPDA Lidar Applications

A highly efficient, versatile, single frequency 2-micron pulsed laser can be used in a pulsed Differential Absorption Lidar (DIAL) / Integrated Path Differential Absorption (IPDA) instrument to make precise, high-resolution measurements to investigate sources and sinks of CO2. For a direct detection IPDA lidar, the desired 2 m Ho:YLF laser should generate 30-40 mJ pulses at the repetition rate of 100 to 200 Hz, with short pulse length (<100 ns) and better than 2% wall plug efficiency. A Tm fiber laser in-band pumped Ho:YLF laser has been developed to meet this technical challenge. This Ho:YLF laser is designed in a four mirror ring resonator with bow tie configuration, which helps to obtain high beam quality. It is end-pumped by a 40 W linearly polarized Tm fiber laser at 1.94μm. The resonator length is 1.10 meters with output coupler reflectivity at 45%. The laser crystal size is 3 x 3 x 60 mm (w, h, l) with a doping concentration of 0.5% Holmium. The laser beam and pump beam are mode-matched in the active medium. Thus, the pump and laser beams have the same confocal parameters. Mode-matching is also helpful for operating the laser in a single transverse mode. The laser beam waist is slightly less than 0.5 mm at the center of the laser crystal. Based on quasi-four level modeling, pump absorption and saturation depend on laser intensity. Laser amplification and saturation also depend on the pump intensity in the crystal. The laser is injection seeded to obtain the single frequency required by an IPDA lidar measurement. The seed beam is entered into the resonator through an output coupler. The laser is mounted on a water cooled optical bench for stable and reliable operation. The size of the optical bench is 22.16 x 9.20 x 1.25 inches. It is stiffened so that the laser can be operated in any orientation of the optical bench. This packaged Ho:YLF laser is designed for either mobile trailer or airborne platform operation. The engineering prototype Ho:YLF laser has been fully characterized to demonstrate laser performance. Figure 1 shows the laser output power as a function of pump power at different pulse repetition rates from 100 Hz to 333 Hz. The threshold of the laser is less than 14 W. The slope efficiencies are 28%, 40%, 41% and 43% for pulse repetition rates of 100, 200, 250 and 333 Hz, respectively. Maximum power increases with the pulse repetition rate. Output power of 4.2 W, 6 W, 6.7 W, and 7.7 W is achieved for pulse repetition rates of 100, 200, 250 and 333Hz, respectively. This represents the optical conversion efficiency of 16.7%, 22.4%, 23.7%, and 26.5% at these various pulse repletion rates. It is the most efficient and compact Ho:YLF laser demonstrated in the high pulse energy (>20mJ) and moderate pulse repetition rate (100's Hz) operation range. As shown in Figure 1, the maximum pulse energy at 100 Hz is 42 mJ. This is limited due to optical damage. The laser stability is characterized and found to be very stable. A relative pulse energy standard deviation of 2% was measured. The beam quality of the Ho:YLF was measured by a Spiricon infrared laser beam camera. Figure 2 shows the beam profile image of the laser. Both the X-profile of the beam (horizontal direction) and the Y-profile of the beam (vertical direction) are well fitted by a Gaussian profile. The qualitative beam quality measurement shows excellent beam quality in both axis. The M-square value for the laser beam is measured at 1.06 and 1.09 for the x and y axis respectively.-

Yu, J.↗
NASA NTRS1990

Growth and characterization of CdS crystals

A growth method for the physical vapor transport of compound semiconductors in closed ampoules is described. With the unique techniques applied in the heat treatment of the starting materials and the temperature profiles provided by the three-zone translational furnace, large crystals of CdS have been grown successfully by the method at lower temperatures than previously used. Both unseeded and seeded growth have been investigated. The CdS crystals were examined using optical and scanning electron microscopies (SEM) to study the microstructure and the dislocation etch-pits. The crystals were further characterized by infrared (IR) and ultraviolet (UV) transmission measurements.

Su, Ching-Hua↗
NASA NTRS1998

Contactless Growth of ZnSe Single Crystals by Physical Vapor Transport

ZnSe crystals were grown by self-seeded physical vapor transport (PVT) technique in the horizontal configuration. The source materials were heat treated by H2 reduction to remove the oxide followed by baking under dynamic vacuum to adjust the source composition toward that of congruent sublimation. Contactless growth of ZnSe single crystals have been performed consistently using three different source materials. The crystals grew away from the wall during the later stage of the growth with large (110) facets tend to align parallel to the gravity direction. The Scanning Electron Micrography (SEM) micrographs and the Atomic Force Microscope (AFM) images showed that large (110) terraces and steps dominate the as-grown facets. The measured residual gas pressures in the processed ampoules agree well among various source materials and the major components were CO and H2. No preferred growth direction was found. The one-dimensional diffusion model on the mass flux of a multi-species PVT system was employed to analyze the conditions for contactless growth. The calculated thermal profile for supersaturation is very close to the thermal profile measured inside the empty furnace bore in the region of contactless growth. The effects of convective flows in the vapor phase inside the ampoule on the growth processes are discussed.

Su, Ching-Hua↗
NASA NTRS2000

Float-Zone Growth of Gel-xSix (x ? 10 at .%) Single Crystals: Influence of Thermocapillary and Solutocapillary Convection

Gel-xSix (x ? 10 at.%) single crystals have been grown with the float-zone technique applied within a monoellipsoid mirror furnace. The feed crystal consisted of synthesized GeO.95siO.05 polycrystalline material. Two Boron-doped (much much more than 1-2 (raised dot) 1017 at/cm3) crystals were grown under identical conditions using <100> Ge seeds. One Ge:Ga-doped (much much more than 1018 at/cm3) reference crystal was also grown in the same furnace. Compositional profiles were measured with an energy dispersive analysis by X-ray (EDAX). The maximum silicon concentration attained was 10 at.%. Micrographs of the etched crystals show sharp changes in interface curvature at the crystal edges. These are considered to be caused by solutal Marangoni convection, whose strength is assumed to be a direct function of silicon concentration, Theoretical considerations show that the flow direction, velocity, and strength varies significantly from a solutal Marangoni convection regime directly in front of the solid-liquid interface to a thermal Marangoni convection regime within the bulk melt.

Campbell, Tom A.↗
NASA NTRS1998

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

Cr-doped ZnSe single crystals were grown by self-seeded physical vapor transport technique under both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. The growth temperatures were in the range of 1140 to 1150C and the furnace translation rates were 1.9 to 2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The different features on the as-grown surface of the vertically and horizontally grown crystals suggests that different growth mechanisms were involved for the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8 to 8.3 x 10(exp 19)/cubic centimeter from optical absorption measurements. The crystalline quality of the grown crystals were examined by high resolution triple crystal X-ray diffraction (HRTXD) analysis.

Su, Ching-Hua↗
NASA NTRS1998

Solution Growth of a Novel Nonlinear Optical Material: L-Histidine Tetrafluoroborate

Single crystals of L-Histidine tetrafluoroborate (L-HFB), a semiorganic nonlinear optical (NLO) material have been successfully grown by the temperature lowering and evaporation methods in our laboratory. Solubility curves of L-HFB have been determined in different solvents, such as water, ethanol and acetone. The solubility of L-HFB is very low in acetone, and ethanol, therefore, it is not feasible to grow L-HFB single crystals using these solvents. Good quality single crystals of a novel nonlinear optical material L-HFB have been grown from aqueous solution. Effects of seed orientation on morphologies of L-HFB crystals were studied. The advantages and disadvantage of both the evaporation and the temperature lowering techniques are compared. The single crystals in size 20 x 20 x 10 cubic mm were grown with deionized water as solvent in two weeks with an approximate growth rate of 1.4mm/day. The transmission range for these crystals has been found to be from 250 nm to 1500 nm.

Aggarwal, M. D.↗
NASA NTRS1991

Stability of Y-Ba-Cu-oxide phases in salt flux

The results of an investigation into the possibility of growing YBa2Cu3O7 (or Y123) single crystals from a NaCl-KCl flux (salt flux) are presented. They are compared with results for Y123 crystals grown from a Ba-Cu-oxide flux system. The chosen salt flux composition was 1:1 (NaCl:KCl). The preparation method of the solutes is presented, with particular attention given to the compounds surrounding the Y123 phase, such as Y2BaCuO6 (Y211). Optical microscopy was introduced to study the morphology of the sample; X-ray diffraction was used for phase identification; and a chemical analysis was effected. The Y123, Y211, and BaCuO2 phases were shown to be dissociated in the NaCl-KCl flux, and could not be recrystallized. A small amount of the flux could be added to create large-grain Y123 crystals, but single-crystal growth was not possible in a top-seeded NaCl-KCl solution. This is attributed to significant differences in solubility of the crystal elements, and phase separation caused by CuO crystal formation.

Tao, Y. K.↗
NASA NTRS1997

Single Crystal Synthesis and STM Studies of High Temperature Superconductors

This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

Barrientos, Alfonso↗
NASA NTRS1999

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.↗
NASA NTRS1999

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

Cr-doped ZnSe single crystals were grown by a self-seeded physical vapor transport technique in both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. Growth temperatures were in the range of 1140-1150 C and the furnace translation rates were 1.9-2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Different features of the as-grown surface of the vertically and horizontally grown crystals suggest that different growth mechanisms were involved in the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8-8.3 x 10 (exp 19) cm (exp -3) from optical absorption measurements. The crystalline quality of the grown crystals were examined by high-resolution triple-crystal X-ray diffraction (HRTXD) analysis.

Su, Ching-Hua↗
NASA NTRS2019

Frequency Control of Multi-Pulse 2-micron Laser Transmitter for Atmospheric Carbon Dioxide Measurement

Laser sources with highly stabilized emission wavelength is of paramount importance for a long term atmospheric carbon dioxide (CO2) measurement from a space platform. Integrated Path Differential Absorption (IPDA) lidar is a promising instrument for such a task. The design of a laser transmitter, with emphasis on the method used to control and select several wavelengths, is presented. This multi-pulsed, injection seeded, 2-μm transmitter uses a Ho:Tm:YLF laser crystal which has matching emission to the absorption of CO2 in the R30 spectroscopic area. The injection seeded laser produces triple single longitudinal mode transform limited line width pulses with a total of 80 mJ at a repetition rate of 50 Hz.

Petros, Mulugeta↗
NASA NTRS1991

Mapping crystal defects with a digital scanning ultramicroscope

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or three dimensional perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometer, which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Springer, J. M.↗
NASA NTRS1993

System performance and on-orbit operations of the Crystal Growth Furnace (CGF) on the first United States microgravity laboratory mission

The paper discusses the design, the performance, and on-orbit operations of the Crystal Growth Furnace (CGF) system flown for the first time aboard the Orbiter Columbia on STS-50. Four experiments were carried out: (1) crystal growth of (Hg,Zn)Te by chemical vapor transport, (2) seeded Bridgman growth of Zn-doped CdTe, (3) Bridgman growth of Se-doped GaAs, and (4) crystal growth of (Hg,Zn)Te by directional solidification. The results of a system performance data analysis demonstrate that all the elements of the CGF system functioned flawlessly. Seven out of eight samples carried on board yielded the best possible science return to date, surpassing previous microgravity material processing experiments in space.

Srinivas, R.↗
NASA NTRS1993

Nd:YLF laser for airborne/spaceborne laser ranging

In order to meet the need for light weight, long lifetime, efficient, short pulse lasers, a diode-pumped, Nd:YLF oscillator and regenerative amplifier is being developed. The anticipated output is 20 mJ per 10 picosecond pulse, running at a repetition rate of 40 Hz. The fundamental wavelength is at 1047 nm. The oscillator is pumped by a single laser diode bar and mode locked using an electro-optic, intra-cavity phase modulator. The output from the oscillator is injected as a seed into the regenerative amplifier. The regenerative amplifier laser crystal is optically pumped by two 60W quasi-cw laser diode bars. Each diode is collimated using a custom designed micro-lens bar. The injected 10 ps pulse from the oscillator is kept circulating within the regenerative amplifier until this nanojoule level seed pulse is amplified to 2-3 millijoules. At this point the pulse is ejected and sent on to a more standard single pass amplifier where the energy is boosted to 20 mJ. The footprint of the entire laser (oscillator-regenerative amplifier-amplifier) will fit on a 3 by 4 ft. optical pallet.

Dallas, Joseph L.↗
NASA NTRS1989

Novel protein crystal growth technology: Proof of concept

A technology for crystal growth, which overcomes certain shortcomings of other techniques, is developed and its applicability to proteins is examined. There were several unknowns to be determined: the design of the apparatus for suspension of crystals of varying (growing) diameter, control of the temperature and supersaturation, the methods for seeding and/or controlling nucleation, the effect on protein solutions of the temperature oscillations arising from the circulation, and the effect of the fluid shear on the suspended crystals. Extensive effort was put forth to grow lysozyme crystals. Under conditions favorable to the growth of tetragonal lysozyme, spontaneous nucleation could be produced but the number of nuclei could not be controlled. Seed transfer techniques were developed and implemented. When conditions for the orthorhombic form were tried, a single crystal 1.5 x 0.5 x 0.2 mm was grown (after in situ nucleation) and successfully extracted. A mathematical model was developed to predict the flow velocity as a function of the geometry and the operating temperatures. The model can also be used to scaleup the apparatus for growing larger crystals of other materials such as water soluble non-linear optical materials. This crystal suspension technology also shows promise for high quality solution growth of optical materials such as TGS and KDP.

Nyce, Thomas A.↗
NASA NTRS2001

The Effect of the Wall Contact and Post-Growth, Cool-Down on Defects in CdTe Crystals Grown By 'Contactless' PVT

To take a maximum advantage of materials processing in microgravity for understanding the effects of gravity, gravity-independent effects should be minimized. In crystal growth, the quality of the grown crystals may depend, among other factors, on their interaction with the walls of the processing container during and after growth, and on the rate of the crystal cool-down at the end of the process. To investigate the above phenomena, a series of CdTe crystal growth processes was carried out. The crystals were grown by physical vapor transport without contact with the side walls of the silica glass ampoules. To eliminate the effect of the seed quality, and to reduce the number of nuclei and related crystal grains, the Low Supersaturation Nucleation technique was applied. The source temperature was 930 C, the undercooling was a few degrees. The crystals, having the diameter of 25 mm, grew at the rate of a few mm per day. The post-growth cool-down to the room temperature was conducted at different rates, and lasted from a few minutes to four days. The crystals were characterized using chemical etching, low temperature luminescence, and Synchrotron White Beam X-ray Topography techniques. The dislocation (etch pit) density was measured and its distribution was analyzed by comparison with Poisson curves and with the Normalized Radial Distribution Correlation Function. In the regions where the crystal is in contact with silica, the materials show a considerable strain field which extends for a few mm or more from the silica-crystal interface. In the reference crystal grown with contact with the ampoule walls, and when the crystals are cooled at the highest rates, the etch pit/dislocation density is in the high 10(exp 5) per square centimeter region. Typical EPD values for lower cool-down rates are in the lower 10(exp 4) per square centimeter region. In some areas the actual dislocation density was about 10(exp 3) per square centimeter or even less. No apparent effect of the cool-down rate on polygonization was observed. Low temperature PL spectra show, that the dominant peak is (D(sup 0), h) and (A(sup 0), e) for samples with low and high dislocation densities, respectively. For low EPD crystals a peak at 1.45 eV with 21 meV phonon replicas was observed and attributed to donor-acceptor pair to neutral copper-acceptor transition. In high EPD crystals this PL structure was not observed, apparently due to the masking effect of the strong contribution from the dislocation band.

Palosz, W.↗
NASA NTRS1985

High-thermal-gradient Superalloy Crystal Growth

Single, (001)-oriented crystals of PWA 1480 were processed in alumina/silica shell molds in a laboratory high gradient furnace. The furnace employs a graphite resistance heated element, a radiation baffle, and a water cooled radiation trap below the baffle. All crystals were grown in vacuum (10 torr) and all heat transfer was radiative. The element is constructed with a variable cross section that is tapered just above the baffle to maximize heat input and therefore thermal gradient. A maximum alloy temperature of 1600 C was used. A thermal gradient of 130 deg C/cm was recorded at 1370 C just above the solidus of the PWA 1480 alloys. Crystal bars with 14.4 and 17.5 mm diameters were grown in alumina/silica shell molds. Each crystal was started from a 1.6 mm pencil seed at a rate of 76 mm/hr and slowly accelerated to a rate of 200 mm/hr under computer control. Volume percent porosity and average pore size were measured as functions of distance in representative bars. Low cycle fatigue behavior and stress rupture properties were determined.

Pearson, D. D.↗
NASA NTRS2010

315mJ, 2-micrometers Double-Pulsed Coherent Differential Absorption Lidar Transmitter for Atmospheric CO2 Sensing

The design of a double pulsed, injection seeded, 2-micrometer compact coherent Differential absorption Lidar (DIAL) transmitter for CO2 sensing is presented. This system is hardened for ground and airborne applications. The design architecture includes three continuous wave lasers which provide controlled on and off line seeding, injection seeded power oscillator and a single amplifier operating in double pass configuration. As the derivative a coherent Doppler wind lidar, this instrument has the added benefit of providing wind information. The active laser material used for this application is a Ho: Tm:YLF crystal operates at the eye-safe wavelength. The 3-meter long folded ring resonator produces energy of 130-mJ (90/40) with a temporal pulse length around 220 nanoseconds and 530 nanosecond pulses for on and off lines respectively. The separation between the two pulses is on the order of 200 microseconds. The line width is in the order of 2.5MHz and the beam quality has an M(sup 2) of 1.1 times diffraction limited beam. A final output energy for a pair of both on and off pulses as high as 315 mJ (190/125) at a repetition rate of 10 Hz is achieved. The operating temperature is set around 20 C for the pump diode lasers and 10 C for the rod. Since the laser design has to meet high-energy as well as high beam quality requirements, close attention is paid to the laser head design to avoid thermal distortion in the rod. A side-pumped configuration is used and heat is removed uniformly by passing coolant through a tube slightly larger than the rod to reduce thermal gradient. This paper also discusses the advantage of using a long upper laser level life time laser crystal for DIAL application. In addition issues related to injection seeding with two different frequencies to achieve a transform limited line width will be presented.

Yu, Jirong↗