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12 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Understanding supercooling mechanism in sodium sulfate decahydrate phase-change material

Salt hydrate-based phase-change materials are considered promising for future heat storage applications in residential heating/cooling systems. Smooth phase transition from the liquid to solid phase and vice versa is essential for effective heat exchanger; however, supercooling in salt hydrates delays the onset of liquid–solid phase transition. We investigate the molecular level mechanism of supercooling in sodium sulfate decahydrate (SSD). SSD is a complex salt hydrate whose properties are governed by electrostatic forces that include pure Coulombic interactions as well as hydrogen bonds. Experimentally, we examine the importance of a nucleator in reducing supercooling temperatures. We investigated the effect of various mass concentrations of a borax nucleator on a decrease of supercooling temperatures. Molecular dynamics simulation techniques are used to obtain a basic understanding of supercooling in SSD. We observe that by introducing borax as a nucleator, there is a decrease in the supercooling temperature before nucleation. Our molecular dynamics simulations show that long-range electrostatics between sodium and sulfate ion pairs and that with polar water molecules is responsible for delayed nucleation in SSD that results in supercooling, and also, dynamics of charged molecules slows down. The lack of crystallization leads to amorphous structures in supercooled SSD.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Alginate–Sodium Sulfate Decahydrate Phase Change Composite with Extended Stability

Here, this study reports on the use of sodium alginate to effectively stabilize sodium sulfate decahydrate (Na 2 SO 4 ∙10H 2 O, SSD) based phase change material (PCM) for application as a thermal energy storage material. Alginate/SSD composite PCMs were prepared by blending SSD with different concentrations of alginate polymer. The resulting composite PCMs demonstrate high phase change enthalpy ~160 J/g and extended cycling stability compared to existing PCM composites. The analysis carried out by optical microscopy, X-ray scattering, and periodic density functional theory (DFT) calculations demonstrated that the stabilization effect was caused by the interplay between ionic and hydrogen bond interactions between the alginate and SSD. Additionally, the variation in mechanical properties of PCM composites with polymer concentrations made it possible to formulate a composite that maintains stable performance after 3D printing. The advanced properties make this composite a promising candidate for application as a thermal energy storage material.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

PHASE CHANGE MATERIAL FOR THERMAL ENERGY STORAGE IN BUILDINGS BASED ON SODIUM SULFATE DECAHYDRATE AND DISODIUM HYDROGEN PHOSPHATE DODECAHYDRATE

The worldwide increasing energy demand and 2050 net zero carbon target urge the globe to solve the energy challenge. Thermal Energy Storage (TES) has received significant attention in recent years as TES can be integrated into heating, ventilation, and air-conditioning systems where the energy would be stored during low-demand times and dispatched during high-demand times, resulting in controlling the peak load and improving energy savings. Material development is an integral part of TES. Salt hydrates are appealing due to cost-effectiveness, low- to no toxicity, and their high melting enthalpy, where energy is stored as latent heat. However, most salt hydrates are prone to incongruent melting (i.e., phase separation upon melting), which results in poor stability and large supercooling. In this study, we produced a highly stable novel energy storage material at a composition of 32 wt% sodium sulfate decahydrate, 52 wt% sodium phosphate dibasic dodecahydrate, 12 wt% milled expanded graphite, and 4 wt% borax. The material has a melting temperature of 28°C and an energy storage capacity of 167 kJ/kg with a supercooling of less than 3°C. The system showed no loss in energy storage performance after 150 cycles. The findings suggest that the novel energy storage material developed in this might be utilized in building heating and cooling applications.

Turnaoglu, Tugba↗
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.↗
DOE OSTI2022

Measurement of Thermal Conductivity in a Supercooled Hydrogel-Salt Complex Near Its Phase Transition

Solid-liquid phase transitions, i.e. solidification processes, have applications in data storage, development of novel thermoelectric materials, cooling of microelectronic substrates and air conditioning condensers. Standard analyses of solidification (Stefan problem) assume constant thermal properties of the solid and liquid sides. It is not known how these properties change across the spatial transition interface, though most studies report a discontinuity in the solid and liquid properties through the transition temperature [1]. When the phase transition releases enthalpy, recent research has shown if the phonon or electron transport time is of the same order of magnitude as the time scale of the atomic transformation, this increases the heat capacity of the solid material at temperatures near the phase transition temperature [2]. A fundamental understanding of the phase transition may help shed light on the molecular origins of supercooling and spontaneous nucleation, which will help with applications involving them. We report studies of supercooling and nucleation of sodium sulfate decahydrate, a salt hydrate which is of recent interest in thermal storage, and of a hydrogel-sodium sulfate complex which shows limited supercooling. We will also report the measurement of their thermal properties during the phase transition process. This will be done with a hot-wire setup which produces small temperature changes of the order of ~1 C.

crystallization, phase transformation, thermal con↗
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.↗
DOE OSTI2024

Stabilizing a low temperature phase change material based on Glaubers salt

The aim of this research is to enhance the performance of Glauber's salt (sodium sulfate decahydrate, SSD) as a phase change material (PCM) for thermal energy storage applications, as well as for shipping of temperature-sensitive materials. The study investigates the effects of modifying SSD with potassium chloride (KCl) and ammonium chloride (NH 4 Cl) to achieve lower phase transition temperatures of between +6 °C and + 13 °C. Sodium polyacrylate (PAAS) is employed as a thickening agent to prevent phase separation, and borax is used as a nucleating agent to suppress supercooling. Various ratios of KCl:NH 4 Cl are tested, and the impact of PAAS concentration on phase segregation is explored. The results show that a 2 wt% concentration of PAAS effectively prevents phase separation. Samples with a KCl:NH 4 Cl ratio of 1:1.83 exhibit stable phase transition behavior and maintain latent heat values within the range of 130–140 J/g after 30 thermal cycles. Maintaining a total KCl and NH 4 Cl proportion of 10 wt% is crucial to achieve the desired lower melting temperature. As a result, the study highlights the significance of thermal cycling in improving the stability of the PCM. The optimized SSD-based eutectic PCM formulations hold promise for applications in the cold chain industry.

25 ENERGY STORAGE↗
DOE OSTI2024

Influence of Carboxymethyl Cellulose as a Thickening Agent for Glauber’s Salt-Based Low Temperature PCM

This work is focused on a novel, promising low temperature phase change material (PCM), based on the eutectic Glauber’s salt composition. To allow phase transition within the refrigeration range of temperatures of +5 °C to +12 °C, combined with a high repeatability of melting–freezing processes, and minimized subcooling, the application of three variants of sodium carboxymethyl cellulose (Na-CMC) with distinct molecular weights (700,000, 250,000, and 90,000) is considered. The primary objective is to optimize the stabilization of this eutectic PCM formulation, while maintaining the desired enthalpy level. Preparation methods are refined to ensure repeatability in mixing components, thereby optimizing performance and stability. Additionally, the influence of Na-CMC molecular weight on stabilization is examined through differential scanning calorimetry (DSC), T-history, and rheology tests. The PCM formulation of interest builds upon prior research in which borax, ammonium chloride, and potassium chloride were used as additives to sodium sulfate decahydrate (Glauber’s salt), prioritizing environmentally responsible materials. The results reveal that CMC with molecular weights of 250 kg/mol and 90 kg/mol effectively stabilize the PCM without phase separation issues, slowing crystallization kinetics. Conversely, CMC of 700 kg/mol proved ineffective due to the disruption of gel formation at its low gel point, hindering higher concentrations. Calculations of ionic concentration indicate higher Na ion content in PCM stabilized with 90 kg/mol CMC, suggesting increased ionic interactions and gel strength. A tradeoff is discovered between the faster crystallization in lower molecular weight CMC and the higher concentration required, which increases the amount of inert material that does not participate in the phase transition. After thermal cycling, the best formulation had a latent heat of 130 J/g with no supercooling, demonstrating excellent performance. This work advances PCM’s reliability as a thermal energy storage solution for diverse applications and highlights the complex relationship between Na-CMC molecular weight and PCM stabilization.

25 ENERGY STORAGE↗
DOE OSTI2026

Determining the Solubility Behavior of Kogarkoite in Simulated Nuclear Waste

Kogarkoite (Na 3 FSO 4 ) is a sparingly soluble fluoride–sulfate double salt that has been identified in high level nuclear waste sludge at the Hanford Site and, more recently, in sludge batch compilation samples at the Savannah River Site (SRS). Due to its complex dissolution behavior, which exhibits an inverse dependence on sodium ion activity, the presence of this mineral poses significant challenges to waste retrieval and processing. Incomplete dissolution during sludge washing can lead to the retention of fluoride and sulfate in the high-level waste feed, potentially causing the formation of corrosive, immiscible molten salt layers, known as "glass gall,” in vitrification melters. Current efforts to optimize flowsheet parameters and wash-water volumes are hindered by the absence of a commercially available, certified reference material, which prevents the accurate calibration of analytical methods and the verification of dissolution kinetics. To address this critical gap, this research focuses on the laboratory synthesis of pure Kogarkoite to serve as a standard for comprehensive solubility and washing performance testing. A coupled synthesis and simulant campaign was executed using an evaporative crystallization protocol designed to replicate the dynamic concentration effects observed in tank farm operations. Thirteen simulant matrices were prepared by dissolving systematically varied ratios of sodium fluoride (NaF) and sodium sulfate (Na 2 SO 4 ) in deionized water under three distinct caustic regimes: 0.0 g (control), 4.0 g (~1 M), and 12.0 g (~3 M) sodium hydroxide (NaOH). While thermodynamic equilibrium models suggest that high-caustic environments should favor the stability of the double salt7, results from this evaporative study at 25 0 C revealed a distinct kinetic divergence. Simulants with high hydroxide loading predominantly yielded large, blocky crystals of sodium sulfate decahydrate (Na 2 SO 4 .10H 2 O). Successful synthesis of pure Kogarkoite was achieved exclusively in specific NaOH-free compositional windows, where the precipitate manifested as fine, opaque granular aggregates. Ion chromatography (IC) analysis confirmed phase purity through the simultaneous stoichiometric depletion of both fluoride and sulfate from the supernatant. This successful synthesis establishes a reproducible route to generate bulk Kogarkoite, enabling the subsequent phase of quantitative dissolution testing using inhibited water to optimize sludge-batch assembly.

Sarker, Md Sharif [Florida International Univ. (FI↗
DOE OSTI2022

Stable salt hydrate-based thermal energy storage materials

Heating and cooling systems in building infrastructure utilize conventional materials that account for a considerable amount of energy usage and waste. Phase change material (PCM) is considered a promising candidate for thermal energy storage that can improve energy efficiency in building systems. In this work, a novel salt hydrate-based PCM composite with high energy storage capacity, relatively higher thermal conductivity, and excellent thermal cycling stability was designed and developed. The thermal cycling stability of the PCM composite was enhanced by using dextran sulfate sodium (DSS) salt as a polyelectrolyte additive, which significantly reduced the phase segregation of salt hydrate. The energy storage capacity and the thermal conductivity of the composite were enhanced by the addition of various graphitic materials along with Borax nucleator. A significant increase in thermal cycling stability was observed for the DSS-modified composite, with over 100 thermal cycles without degradation. The final PCM composite exhibited as much as 290% increase in energy storage capacity relative to the pure salt hydrate, and approximately 20% increase in thermal conductivity. In addition, the PCM composite developed can be produced at larger scale, and can potentially change the future of heating/cooling system in building infrastructure.

42 ENGINEERING↗