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DOE OSTI2022

Electrodeposited Sn–Cu@Sn dendrites for selective electrochemical CO 2 reduction to formic acid

Large-scale CO 2 electrolysis can be applied to store renewable energy in chemicals. Recent developments in gas diffusion electrodes now enable a commercially relevant current density. However, the low selectivity of the CO 2 reduction reaction (CO 2 RR) still hinders practical applications. The selectivity of the CO 2 RR highly depends on the electrocatalyst. Sn catalysts are considered promising cathode materials for the production of formic acid. The selectivity of Sn catalysts can be regulated by controlling their morphology or alloying them with secondary metals. In this work, we enhanced the selectivity of CO 2 reduction to formic acid by synthesizing Sn–Cu@Sn dendrites that have a core@shell architecture. The Sn–Cu@Sn dendrites were prepared by a scalable electro-deposition method. The electronic structure was modified to suppress a reaction pathway for CO production on the Sn surface. Notably, the Sn shell inhibited the cathodic corrosion of Cu during the CO 2 RR. On a gas diffusion electrode, the Sn–Cu@Sn dendrites exhibited 84.2% faraday efficiency to formic acid for 120 h with high stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

New Empirical Formulation for the Sublimational Breakup of Graupel and Dendritic Snow

Abstract Ice fragments are generated by sublimation of ice particles in subsaturated conditions in natural clouds. Conceivably, such sublimational breakup would be expected to cause ice multiplication in natural clouds. Any fragment that survives will grow to become ice precipitation that may sublimate and fragment further. As a first step toward assessing this overlooked process, a formulation is proposed for the number of ice fragments from sublimation of ice particles for an atmospheric model. This is done by amalgamating laboratory observations from previously published studies. The concept of a “sublimated mass activity spectrum” for the breakup is applied to the dataset. The number of ice fragments is determined by the relative humidity over ice and the initial size of the parent ice particles. The new formulation applies to dendritic crystals and heavily rimed particles only. Finally, a thought experiment is performed for an idealized scenario of subsaturation with in-cloud descent. Scaling analysis yields an estimate of an ice enhancement ratio of about 5 (10) within a weak deep convective downdraft of about 2 m s −1 , for an initial monodisperse population of dendritic snow (graupel) particles of 3 L −1 and 2 mm. During descent, there is a dynamic equilibrium between continual emission of fragments and their depletion by sublimation. A simplified bin microphysics parcel model exhibits this dynamical quasi equilibrium, consistent with the thought experiment. The fragments have average lifetimes of around 90 and 70 s for dendrites and graupel, respectively. Sublimational breakup is predicted to cause significant secondary ice production.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Dendritic microstructures observed in electron-beam deposited hafnia films

Dendritic microstructures inside hafnia dielectric coatings fabricated via electron-beam deposition are investigated. These structures are observable with different optical characterization tools, including atomic force microscopy, fluorescence microscopy, Raman microscopy, and differential interference contrast microscopy. Long-term monitoring of individual samples over a seven-year time span revealed that the dendrite-like structures evolve over time, while the hafnia material in the dendrite structure—as compared to the rest of the coating—shows a decrease in crystallinity and an increase in defect density.

Hoffman, B. N. [Univ. of Rochester, NY (United Sta↗

NASA NTRS1979

Influence of convection on free growth of dendrite crystals from solution

The free growth of dendrites in a uniformly supercooled solution was examined using cine photography with a Schlieren optical system. Crystals were grown in the bulk of the solution from a centrally located capillary tube, nucleated at the interface with a liquid nitrogen cooled wire. Crystals propagated along the tube, the slower growing orientations eliminated, and emerged at the tip, usually growing parallel to the tube direction. For both sodium sulfate decahydrate from its solution and ice from sodium chloride solution, growth rate and fineness of dendrites increased with supercooling. In sodium sulfate, upward convection of the less dense depleted solution occurs; downward convection was observed for the rejected, more concentrated sodium chloride solution. In both cases, there was a spatial and temporal delay in the release of the convective plume from the moving dendrite tip. The role of this convection on the growth characteristics and the production of secondary crystals is examined. A proposed low-g experiment to examine differences in growth rate, crystal texture, and secondary nucleation in a reduced convective regime where molecular diffusion is the dominant transfer process is discussed.

Hallett, J.↗

NASA NTRS1982

The influence of acceleration forces on dendritic growth and grain structure

The results of experiments on the tin-15 wt pct lead system are presented, showing the effects on microstructure of solidification in the presence of acceleration forces from 0.0001 to 5 g for three cooling rates. An increase in the acceleration level is shown to drive fluid flow and cause dendrite remelting, fragmentation, and macrosegregation. The cooling rate impacts the final structure through its control of dendrite arm spacings and permeability to fluid flow. At the low (0.0001 g) acceleration, dendrite arm spacings deviated from the predicted relationship to cooling rate. An explanation for this anomaly is given which considers the temperature and concentration gradients in the low-gravity environment.

Johnston, M. H.↗

NASA NTRS1983

Gravitational effects in dendritic growth

The theories of diffusion-controlled dendritic crystallization will be reviewed briefly, along with recently published critical experiments on the kinetics and morphology of dendritic growth in pure substances. The influence of the gravitational body force on dendrite growth kinetics will be shown to be highly dependent on the growth orientation with respect to the gravity vector and on the level of the thermal supercooling. In fact, an abrupt transition occurs at a critical supercooling, above which diffusional transport dominates the growth process and below which convective transport dominates. Our most recent work on binary mixtures shows that dilute solute additions influence the crystallization process indirectly, by altering the interfacial stability, rather than by directly affecting the transport mode. Directions for future studies in this field will also be discussed.

Glicksman, M. E.↗

NASA NTRS1984

Emitter formation in dendritic web silicon solar cells

The use of liquid dopants and liquid masks for p-n junction formation in dendritic web solar cells was investigated and found to be equivalent to the use of gaseous dopants and CVD SiO2 masks previously used. This results in a projected cost reduction of 0.02 1980$/Watt for a 25 MW/year production line, and makes possible junction formation processes having a higher throughput than more conventional processes. The effect of a low-energy (0.4 keV) hydrogen ion implant on dendritic web solar cells was also investigated. Such an implant was observed to improve Voc and Jsc substantially. Measurements of internal quantum efficiency suggest that it is the base of the cell, rather than the emitter, which benefits from the hydrogen implant. The diffusion length for electrons in the p-type base increased from 53 microns to 150 microns in one case, with dendritic web cell efficiency being boosted to 15.2 percent. The mechanism by which low-energy hydrogen ions can penetrate deeply into the silicon to effect the observed improvement is not known at this time.

Meier, D. L.↗

NASA NTRS1984

Dendritic solidification in a binary alloy melt: Steady-state versus morphological stability theories

A model for dendritic growth in a binary alloy melt, in the presence of a positive temperature gradient in the liquid, is presented. The model describes satisfactorily the transition from a dendritic interface to a planar interface at very low and very large growth rates. A dendrite tip stability parameter is derived, strictly from steady state considerations, without resorting to a perturbation analysis. The estimates of the parameter agree with those obtained by models based on perturbation analyses.

Laymanan, V.↗

NASA NTRS1986

The effect of fluid flow due to the crystal-melt density change on the growth of a parabolic isothermal dendrite

The Ivantsov (1947) analysis of an isolated isothermal dendrite (with zero surface tension) growing into a supercooled liquid is extended to include the effects of the fluid flow due to volume contraction or expansion upon solidification. For an axisymmetric paraboloidal dendrite, an analytic solution to the Navier-Stokes equations is obtained. The magnitude of the flow is proportional to the relative density change epsilon, and the flow becomes negligible far from the surface of the dendrite. The temperature field consistent with this flow can also be found explicitly. The well-known expression that relates the dimensionless supercooling to the Peclet number in the absence of fluid flow is modified for nonzero epsilon, but the effect is of order epsilon and hence is seen to be minor for most values of epsilon and dimensionless supercooling that occur in practice.

Mcfadden, G. B.↗

NASA NTRS1987

A critical examination of the dendrite growth models Comparison of theory with experimental data

Three dendrite growth models for directionally solidified succinonitrile-acetone, succinonitrile-salol, aluminum-copper, and lead-paladium alloys are evaluated. The characteristics of the Burden and Hunt (1974) model, the Laxmanan (1985) model, and the Trivedi (1980) model are described. The dendrite tip temperature, tip radius, liquid composition, and primary arm spacing for the alloys are analyzed in terms of growth speed, alloy composition, and temperature gradient. It is observed that the Burden and Hunt model accurately predicts the proper behavior of the parameters, but does not provide good quantitative predictions. A good fit between the experimental data and the Trivedi and Laxmanan models is detected. The advantages of the Trivedi marginal stability analysis and the Laxmanan minimum dendrite tip undercooling approaches are discussed.

Tewari, S. N.↗

NASA NTRS1987

Dendritic growth of undercooled nickel-tin. I, II

A comparison is made between high speed cinematography and optical temperature measurements of the solidification of an undercooled Ni-25 wt pct Sn alloy. The first part of this study notes that solidification during the recalescence period at all undercoolings studied occurred in the form of a dendritelike front moving across the sample surface, and that the growth velocities observed agree with calculation results for the dendrite growth model of Lipton et al. (1986); it is concluded that the coarse structure observed comprises an array of much finer, solute-controlled dendrites. In the second part, attention is given to the solidification of levitated metal samples within a transparent glass medium for the cases of two undercooled Ni-Sn alloys, one of which is eutectic and another hypoeutectic. The data obtained suggest a solidification model involving dendrites of very fine structure growing into the melt at temperatures near the bulk undercooling temperature.

Wu, Y.↗

NASA NTRS1986

Dendrite characteristics in directionally solidified Pb-8 pct Au and Pb-3 pct Pd alloys

An investigation of Pb-8 pct Au and Pb-3 pct Pd alloy specimens which have been partially directionally solidified and then quenched is performed in order to characterize their dendritic microstructural details and solute composition profiles. A controlled sectioning technique is employed to measure dendrite tip radii. It is found that most of the observed behavior is predicted quite well by a modification of the Burden and Hunt (1974) model proposed by Laxmanan (1984), in addition to the models based on the marginal stability approach. Results indicate that quantitative comparison of the primary arm spacing measurements can not form the basis of distinguishing among the various dendrite growth models in a positive temperature gradient.

Tewari, S. N.↗

NASA NTRS1987

On the role of convective motion during dendrite growth: Experiments under variable gravity, revised

Experiments show the effect of self induced convection on individual dendrite growth in uniformly supercooled samples and solidification of the resulting mush under conditions of high and low g. Convection is visualized by a Schlieren optical system or a Mach Zender interferometer. For ice crystals growing from the vapor in air, a slight reduction in linear growth rate occur under low g. For ice crystals growing from NaCl solution, dendrite tip velocities are unchanged, but subsequent mush solidification is enhanced through drainage channels under higher g. By contrast, sodium sulfate decahydrate dendrites growing from solution produce convective plumes which lead to higher tip growth rate only as the crystal growth direction approaches that of gravity. Convective plumes are laminar for small crystals under conditions of these experiments; the rise velocity of such plumes is greater than individual vortex rings under identical conditions. Convection effects are only present in solution under a critical supercooling less than about 5 C for sodium sulfate and 2 C for ice in NaCl since at higher supercooling the crystallization velocity, proportional to the square of the supercooling, exceeds the convective velocity, proportional to the square root of the supercooling. The role of convective velocity in bulk solidification is to give a large scale flow which under extreme cases may lead to extensive secondary crystal production, which alters the resulting crystal texture of the completely solidified melt.

Hallett, J.↗

NASA NTRS1988

Dendritic growth in the presence of convection

The motion of the freezing front between a dendritic crystal and a supercooled liquid is studied using an interface evolution equation derived from a boundary integral transformation of the transient convective-diffusion equation. A new steady-state theory is introduced that incorporates the effects of convection in dendritic growth. It is shown that in the absence of capillary effects the shape of the crystal-melt interface is a paraboloid of revolution, similar to that found in situations where diffusion is the sole heat transfer mechanism. A relation between the supercooling, the product of the tip velocity and tip radius, and the strength of the flow is derived which reduces to the well-known Ivantsov theory in the absence of convection. A non-linear interface-tracking algorithm is developed and used to study the temporal and spatial evolution of the dendritic interface. The important role of capillarity and convection on the interface dynamics is established and the response of the interface to finite amplitude disturbances is examined for the first time. Tip splitting is identified as the dominant destabilization mechanism in the limit of zero surface tension. Finite surface tension leads to interface stabilization, irrespective of the magnitude and structure of the external perturbations. Finally, convection significantly decreases the magnitude of the freezing velocity.

Beaghton, Pantelis John↗

NASA NTRS1988

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.↗

NASA NTRS1987

Isothermal dendritic growth - A low gravity experiment

The Isothermal Dendritic Growth Experiment has been designed to test dendritic growth theory at low undercoolings, under microgravity conditions in the Space Shuttle Cargo Bay-borne Material Science Laboratory. The experiment will be essentially autonomous, although limited in-flight interaction through a computer interface is planned. A crystal growth chamber able to yield oriented single-crystal dendritic growth will be incorporated; 'seeding' the chamber with a crystal of the requisite orientation will not in itself meet this requirement.

Glicksman, M. E.↗

NASA NTRS1987

Solidification under microgravity conditions - Dendritic growth

The experimental approach and apparatus of a zero-gravity active crystal growth experiment to test dendritic growth theory at low supercoolings are discussed. The experiment consists of 20 experimental cycles. Estimates have been made as to how low gravitational accelerations would have to be reduced to observe convection-free dendritic growth at supercoolings from 0.01-1.0 K. The experiment requires temperature control of + or - 2 mK and photographic resolution of a few microns with a depth of field of + or - 6 mm. The thermostatic bath and temperature control system, photographic system, growth chamber, and dendrite detection system are described in detail.

Glicksman, M. E.↗

NASA NTRS1988

Isothermal dendritic growth: A low gravity experiment

The Isothermal Dendritic Growth Experiment is an active crystal growth experiment designed to test dendritic growth theory at low undercoolings where convection prohibits such studies at 1 g. The experiment will be essentially autonomous, though limited in-flight interaction through a computer interface is planned. One of the key components of the apparatus will be a crystal growth chamber capable of achieving oriented single crystal dendritic growth. Recent work indicates that seeding the chamber with a crystal of the proper orientation will not, in and of itself, be sufficient to meet this requirement. Additional flight hardware and software required for the STS flight experiment are currently being developed at NASA Lewis Research Center and at Rensselaer Polytechnic Institute.

Glicksman, M. E.↗