Search NASA⌕ Search

SEARCH · Search NASA

Results for “drying methods”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 325 records · Page 18
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Performing In Situ Closed-Cell Gas Reactions in the Transmission Electron Microscope

Gas reactions studied by in situ electron microscopy can be used to capture the real-time morphological and microchemical transformations of materials at length scales down to the atomic level. In situ closed-cell gas reaction (CCGR) studies performed using (scanning) transmission electron microscopy (STEM) can separate and identify localized dynamic reactions, which are extremely challenging to capture using other characterization techniques. For these experiments, we used a CCGR holder that utilizes microelectromechanical systems (MEMS)-based heating microchips (hereafter referred to as "E-chips"). The experimental protocol described here details the method for performing in situ gas reactions in dry and wet gases in an aberration-corrected STEM. This method finds relevance in many different materials systems, such as catalysis and high-temperature oxidation of structural materials at atmospheric pressure and in the presence of various gases with or without water vapor. Here, several sample preparation methods are described for various material form factors. During the reaction, mass spectra obtained with a residual gas analyzer (RGA) system with and without water vapor further validates gas exposure conditions during reactions. Integrating an RGA with an in situ CCGR-STEM system can, therefore, provide critical insight to correlate gas composition with the dynamic surface evolution of materials during reactions. In situ/operando studies using this approach allow for detailed investigation of the fundamental reaction mechanisms and kinetics that occur at specific environmental conditions (time, temperature, gas, pressure), in real-time, and at high spatial resolution.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗
NASA NTRS2022

Trash-to-Gas: Trash Preparation and Feed Mechanism

One method of reducing the mass and volume of astronaut waste items during future exploration missions is a process called Trash-to-Gas (TtG), which uses thermal degradation to convert various astronaut waste items into a gas that can either be repurposed onboard or safely vented overboard. This project aims to determine which methods for pre-processing waste may enhance the gasification efficiency within a microgravity TtG reactor. Preparation methods that were investigated include mixing, pre-drying, shredding, compacting, and raw unprocessed waste. Each of these preparation methods was tested within the state-of-the-art subscale TtG system, known as the Orbital Syngas/Commodity Augmentation Reactor (OSCAR), and the resulting solid-to-gas conversion and burn durations were compared. Full-scale CAD models of these various preparation methods in conjunction with a projected full-scale TtG reactor were created using Creo Parametric. An Equivalent System Mass (ESM) analysis was then performed to trade the benefits of improved solid-to-gas performance with the costs associated with implementing the additional components that would increase system mass, power, volume, and design complexity. The results of this ESM analysis will be leveraged for future full-scale TtG system development to help reduce the overall mass, power, and volume of the system while ensuring effective reactor performance.

Ray Pitts↗
DOE OSTI2023

Insights into the Chemistry of the Cathodic Electrolyte Interphase for PTFE-Based Dry-Processed Cathodes

Dry processing is a promising method for high-performance and low-cost lithium-ion battery manufacturing which uses polytetrafluoroethylene (PTFE) as a binder. However, the electrochemical stability of the PTFE binder in the cathodes and the generated chemistry of the cathode electrolyte interphase (CEI) layers are rarely reported. In this work, the CEI properties and PTFE electrochemical stability are studied via cycling the high-loading dry-processed electrodes in electrolytes with LiPF 6 or LiClO 4 salt. Using LiClO 4 salt can eliminate other possible F sources, allowing the decomposition of PTFE to be studied. The detection of LiF in cells with the LiClO 4 salt confirms that PTFE undergoes side reaction(s) in the cathodes. When compared with LiClO 4 , the CEI layer is much thicker when LiPF 6 is used as the electrolyte salt. These results provide insights into the CEI layer and may potentially enlighten the development of binders and electrolytes for the high efficiency and long durability of DP-based LIBs.

25 ENERGY STORAGE↗
DOE OSTI2012

Impact of Standing Bleed Water on Saltstone Placement

The amount of water present during placement and subsequent curing of saltstone has the potential to impact several properties important for grout quality. An active drain water system can remove residual standing water and expose the surface of the placed saltstone to air. Oxidation of the saltstone may result in an increase in the leachability of redox sensitive elements. A dry surface can lead to cracking, causing an increase in hydraulic conductivity. An inactive drain water system can allow standing water that generates unnecessary hydrostatic head on the vault walls. Standing water that cannot be removed via the drain system will be available for potential incorporation into subsequent grout placements. The objective of this work is to study the impact of standing water on grout quality pertaining to disposal units. A series of saltstone mixes were prepared, and cured at ambient temperature to evaluate the impact of standing water on saltstone placement. The samples were managed to control drying effects on leachability by either exposing or capping the samples. The water to premix ratio was varied to represent a range of processing conditions. Samples were analyzed for density, leachability, and hydraulic conductivity. A monolith of each composition was cut into four sections to analyze the homogeneity of the sample with respect to vertical position within the sample. The density of each section was measured by two methods, helium pycnometry and by ASTM 642-06. The results show a trend of increasing density with increasing depth in the samples. This effect is more pronounced with the inclusion of excess bleed water and indicative of increased settling. The leachability of the eight different samples was analyzed by ANS/ANSI 16.1 method. These results indicate that drying of the saltstone during curing leads to decreased Leachability Indices (indicative of more release) for potassium, sodium, rhenium, nitrite, and nitrate. This may be caused by shrinkage cracking in the samples creating additional pathways for contaminant release. There was no noticeable effect on leachability by changing the water to premix ratio or by including excess bleed water. There was no detectable chromium release in any of the samples. Chromium and rhenium were added in equal amounts to determine whether rhenium might be an acceptable surrogate for chromium, a hazardous material. This testing shows no correlation between the behavior of the two elements, as chromium is not released at detectable levels and rhenium is released at a comparable rate to nitrate, the most prevalent and mobile species in saltstone.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Aerosol-Assisted Deposition for TiO 2 Immobilization on Photocatalytic Fibrous Filters for VOC Degradation

Atomization and spraying are well-established methods for the production of submicrometer- and micrometer- sized powders. In addition, they could be of interest to the immobilization of photocatalytic nanoparticles onto supports because they enable the formation of microporous films with photocatalytic activity. Here, we provide a comparison of aerosol-assisted immobilization methods, such as spray-drying (SD), spray atomization (SA), and spray gun (SG), which were used for the deposition of TiO 2 dispersions onto fibrous filter media. The morphology, microstructure, and electronic properties of the structures with deposited TiO 2 were characterized by SEM and TEM, BET and USAXS, and UV-Vis spectrometry, respectively. The photocatalytic performances of the functionalized filters were evaluated and compared to the benchmark dip-coating method. Our results showed that the SG and SA immobilization methods led to the best photocatalytic and operational performance for the degradation of toluene, whereas the SD method showed the lowest degradation efficiency and poor stability of coating. We demonstrated that TiO2 sprays using the SG and SA methods with direct deposition onto filter media involving dispersed colloidal droplets revealed to be promising alternatives to the dip-coating method owing to the ability to uniformly cover the filter fibers. In addition, the SA method allowed for fast and simple control of the coating thickness as the dispersed particles were continuously directed onto the filter media without the need for repetitive coatings, which is common for the SG and dip-coating methods. Our study highlighted the importance of the proper immobilization method for the efficient photocatalytic degradation of VOCs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Surfactant templated biogenic nanoporous silica thermal insulation composite

Carbon-sequestration biogenic insulation materials offer a promising solution for sustainable and energy-efficient buildings. However, minimizing energy-intensive manufacturing processes and ensuring a uniform microstructure are essential to achieve widespread application. In this work, we introduce cetyltrimethylammonium bromide (CTAB) surfactant as both synthesis and dispersion template for nanoporous silica to create biogenic straw-based thermal insulation composites. As the amount of nanoporous silica increases to 72 wt%, the elastic insulation composite dried using the solvent exchange method exhibits a density of 0.058 g cm –3 , a thermal conductivity of 30.3 mW m –1 K –1 and a flexural modulus of 3.96 MPa, while demonstrating materials circularity and fire retardance. The use of CTAB surfactant effectively captures nanoporous silica, preventing its loss during manufacturing and enhancing the homogeneity and dispersion of the silica within the composite. In addition, the results show that the ethanol solvent exchange drying at ambient conditions provides the optimum thermal insulation performance with less energy consumption compared to freeze-drying.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microbiomes Associated With Foods From Plant and Animal Sources

Food microbiome composition impacts food safety and quality. The resident microbiota of many food products is influenced throughout the farm to fork continuum by farming practices, environmental factors, and food manufacturing and processing procedures. Currently, most food microbiology studies rely on culture-dependent methods to identify bacteria. However, advances in high-throughput DNA sequencing technologies have enabled the use of targeted 16S rRNA gene sequencing to profile complex microbial communities including non-culturable members. In this study we used 16S rRNA gene sequencing to assess the microbiome profiles of plant and animal derived foods collected at two points in the manufacturing process; post-harvest/pre-retail (cilantro) and retail (cilantro, masala spice mixes, cucumbers, mung bean sprouts, and smoked salmon). Our findings revealed microbiome profiles, unique to each food, that were influenced by the moisture content (dry spices, fresh produce), packaging methods, such as modified atmospheric packaging (mung bean sprouts and smoked salmon), and manufacturing stage (cilantro prior to retail and at retail). The masala spice mixes and cucumbers were comprised mainly of Proteobacteria, Firmicutes, and Actinobacteria. Cilantro microbiome profiles consisted mainly of Proteobacteria, followed by Bacteroidetes, and low levels of Firmicutes and Actinobacteria. The two brands of mung bean sprouts and the three smoked salmon samples differed from one another in their microbiome composition, each predominated by either by Firmicutes or Proteobacteria. These data demonstrate diverse and highly variable resident microbial communities across food products, which is informative in the context of food safety, and spoilage where indigenous bacteria could hamper pathogen detection, and limit shelf life.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2021

Pore-scale simulation of drying in porous media using a hybrid lattice Boltzmann: pore network model

In this work, a hybrid method coupling a pseudo-potential lattice Boltzmann model (LBM) and a pore network model (PNM) to simulate drying in porous media is proposed. Based on the watershed method, the porous medium is firstly decomposed into pore regions. According to the liquid–vapor phase distribution at a given time, the pore regions are further divided into four pore types, namely two-phase pores where a liquid–vapor interface exists, buffer pores next to the two-phase pores, single-liquid and single-vapor phase pores. The pseudo-potential LBM is used in the two-phase and buffer pores to simulate liquid drying and track the movement of the interfaces, while the single-phase PNM simulations are conducted in the buffer and single-phase pores to simulate vapor or liquid flow. LBM and PNM are coupled in the buffer pores through exchange of boundary information. The hybrid method is applied to simulate liquid drying in a porous medium. The whole-domain LBM simulation is considered as the reference solution to validate the hybrid method. Liquid saturation variation during the drying process and detailed phase and pressure distributions obtained by the two methods match quite well, demonstrating the accuracy of the hybrid method. For the specific case studied, the hybrid method saves more than 60% computational time compared to the whole-domain LBM simulation. In addition, the speedup of the hybrid method becomes more significant for a larger computational domain. In summary, the hybrid method developed in this work combines the accuracy of LBM and the efficiency of PNM to simulate drying in porous media at pore scale and can lead to significant reduction of computation time, thus allowing the pore-scale consideration of drying in larger porous systems.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Remote Monitoring for Stress Corrosion Cracking in Dry Cask Storage Systems

Acoustic Emission monitoring is a technique that detects and records phenomena related to the elastic waves generated by the release of strain energy during crack propagation events. The sensors used for this method are highly sensitive and do not typically need to be in relatively close proximity to the indication when compared to methods such as ultrasonic or eddy current testing. This characteristic makes acoustic emission an attractive method for monitoring locations that are not readily accessible to active inspection methods, such as with in-situ examination of dry cask storage system canisters. Acoustic emission is unique among nondestructive evaluation (NDE) methods as emission is caused by the energy released from the object inspected. Most NDE methods require that energy be introduced to the part from an external source; which is not necessary with acoustic emission. Acoustic emission signals are created during crack growth and plastic deformation. EPRI has been investigating the feasibility of using acoustic emission as a complementary NDE method for monitoring the structural condition of dry fuel storage canisters. To assess this feasibility three first of a kind field trials were conducted over a one year period. The goals of the field trials were to determine the potential path forward for the method and to assess needs for further research and development. Why this matters: The study evaluated the efficacy of structural health monitoring methods to support ISFSI license renewal commitments to support aging management of welded stainless steel canisters. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Fabric properties and electric efficiency limits of mechanical moisture extraction from fabrics

Residential clothes drying consume about 650 TBtu of primary energy per year in the United States, equivalent to 3% of primary residential energy consumption. There is a strong impetus to reduce the energy consumption of clothes dryers by both improving existing technology and developing alternatives that use fundamentally different drying mechanisms. Clothes drying technologies are broadly classified into either evaporative or mechanical drying. The focus of this paper is on mechanical drying, including vibrational, centrifugal, and press-based methods. In this work, the physical processes involved in these mechanical fabric drying processes were analyzed to develop general theories of mechanical cloth drying energy efficiency. Quantitative evaluation of the theories requires measured fabric properties. To accomplish this, a set of experiments was conducted on samples of a standard test fabric. The fabric was a cotton-polyester blend specified by the US Department of Energy to evaluate the standardized efficiency of all residential clothes dryers in the US. Mercury porosimetry experiments were conducted to determine the fabric pore size distribution, apparent density, and porosity. Elasticity experiments were conducted to determine the fabric’s Young’s modulus. Isostatic press experiments were conducted to establish a relationship between compression force and fabric moisture content. The data resulting from these experiments were combined with mathematical models developed in this work to calculate the theoretical maximum performance limits for mechanical drying of the standard fabric. The results of the analysis are used to make recommendations for the most promising technologies that offer the greatest potential energy savings for residential clothes drying.

36 MATERIALS SCIENCE↗
NASA NTRS2003

A Method of Estimating Transient-Cavity Diameters for Impact Craters Formed in Dry Sand

Analyses of impact craters formed in laboratory experiments historically have been the source of many fundamental observations and interpretations of the impact-cratering process itself. Due to its ready availability, ease of handling, and lack of strength, dry sand of various types has been the target material of choice in the majority of such experiments. A consequence of its lack of intrinsic strength, however, is dry sand's inability to maintain slopes above its angle of repose. Evidence from field observations of simple terrestrial craters and laboratory craters formed in more cohesive granular media suggests that transient cavities are similar to paraboloids in shape. Cross-sections of craters formed in dry sand, however, are nearly conical with the wall slopes at or near the angle of repose, indicating that the original crater form has been modified by one or more processes, among which is simple slope failure. Because the dimensions and shape of the transient cavity reflect the detailed conditions of a given impact event, its characterization has long been a desired goal in experimentation. A means of estimating the position of the transient cavity's rim is suggested below, relying on determination of velocities of material ejected from the growing cavity.

Cintala, M. J.↗
DOE OSTI2014

SU-E-T-106: Development of a Collision Prediction Algorithm for Determining Problematic Geometry for SBRT Treatments Using a Stereotactic Body Frame

Purpose: Collision between the gantry and the couch or patient during Radiotherapy is not a common concern for conventional RT (static fields or arc). With the increase in the application of stereotactic planning techniques to the body, collisions have become a greater concern. Non-coplanar beam geometry is desirable in stereotatic treatments in order to achieve sharp gradients and a high conformality. Non-coplanar geometry is less intuitive in the body and often requires an iterative process of planning and dry runs to guarantee deliverability. Methods: Purpose written software was developed in order to predict the likelihood of collision between the head of the gantry and the couch, patient or stereotatic body frame. Using the DICOM plan and structures set, exported by the treatment planning system, this software is able to predict the possibility of a collision. Given the plan's isocenter, treatment geometry and exterior contours, the software is able to determine if a particular beam/arc is clinically deliverable or if collision is imminent. Results: The software was tested on real world treatment plans with untreatable beam geometry. Both static non-coplanar and VMAT plans were tested. Of these, the collision prediction software could identify all as having potentially problematic geometry. Re-plans of the same cases were also tested and validated as deliverable. Conclusion: This software is capable of giving good initial indication of deliverability for treatment plans that utilize complex geometry (SBRT) or have lateral isocenters. This software is not intended to replace the standard pre-treatment QA dry run. The effectiveness is limited to those portions of the patient and immobilization devices that have been included in the simulation CT and contoured in the planning system. It will however aid the planner in reducing the iterations required to create complex treatment geometries necessary to achieve ideal conformality and organ sparing.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2011

Recovery of Iron/Iron Oxide Nanoparticles from Solution: Comparison of Methods and their Effects

Most methods currently being used to recover Fe0-core/oxide-shell nanoparticles from solutions (including the solvents they are synthesized or stored in) are potentially problematic because they may alter the particle composition (e.g., depositing salts formed from solutes) or leave the particles prone to transformations during subsequent storage and handling (e.g., due to residual moisture). In this study, several methods for recovery of nanoparticles from aqueous solution were studied to determine how they affect the structure and reactivity of the recovered materials. Simple washing of the nanoparticles during vacuum filtration (i.e., “flash drying”) can leave up to ~17 weight percent residual moisture. Modeling calculations suggest this moisture is mostly capillary or matric water held between particles and particle aggregates, which can be removed by drying for short periods at relative vapor pressures below 0.9. Flash drying followed by vacuum drying, all under N2, leaves no detectable residue from precipitation of solutes (detectable by X-ray photoelectron spectroscopy, XPS), no significant changes in overall particle composition or structure (determined by transmission electron microscopy, TEM), and negligible residual moisture (by thermogravimetric analysis, TGA). While this improved flash-drying protocol may be the preferred method for recovering nanoparticles for many purposes, we found that Fe0-core/oxide-shell nanoparticles still exhibit gradual aging during storage when characterized electrochemically with voltammetry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Modeling the Moisture Content and Dry Matter Loss in Dynamic Woody Biomass Storage Piles with Variable Extraction

The urgent need to mitigate climate change has spurred significant interest in renewable energy sources. This paper explores the storage and processing of woody biomass for biofuel production, considering the dynamic nature of biomass piles in real-world scenarios. A model has been developed to analyze moisture content changes and dry matter loss in woody biomass stored in piles prior to processing, taking into account varying extraction methods and environmental conditions. Case studies that examine the effects of different unpiling methods (FIFO, LIFO, and homogeneous) on moisture content and dry matter loss under various feedstock arrival rates and weather conditions are presented. Results indicate that unpiling methods significantly impact moisture content, with LIFO typically resulting in higher moisture content due to the utilization of fresher feedstock. Dry matter loss increases with pile size and time, emphasizing the importance of accurate modeling for assessing carbon emissions and feedstock quality. Furthermore, the model highlights the importance of process loading order and extraction methods in biomass storage, suggesting potential cost benefits associated with decreased moisture content. The difference between different extraction methods could vary the moisture content in the feedstock reaching the biofuel process by as much as 37.6%, however dry matter loss varies minimally for realistic pile changes. Overall, this research contributes to a better understanding of biomass storage dynamics and informs sustainable biofuel production practices.

Niska, Janel↗
DOE OSTI2014

An AFM-based pit-measuring method for indirect measurements of cell-surface membrane vesicles

Highlights: • Air drying induced the transformation of cell-surface membrane vesicles into pits. • An AFM-based pit-measuring method was developed to measure cell-surface vesicles. • Our method detected at least two populations of cell-surface membrane vesicles. - Abstract: Circulating membrane vesicles, which are shed from many cell types, have multiple functions and have been correlated with many diseases. Although circulating membrane vesicles have been extensively characterized, the status of cell-surface membrane vesicles prior to their release is less understood due to the lack of effective measurement methods. Recently, as a powerful, micro- or nano-scale imaging tool, atomic force microscopy (AFM) has been applied in measuring circulating membrane vesicles. However, it seems very difficult for AFM to directly image/identify and measure cell-bound membrane vesicles due to the similarity of surface morphology between membrane vesicles and cell surfaces. Therefore, until now no AFM studies on cell-surface membrane vesicles have been reported. In this study, we found that air drying can induce the transformation of most cell-surface membrane vesicles into pits that are more readily detectable by AFM. Based on this, we developed an AFM-based pit-measuring method and, for the first time, used AFM to indirectly measure cell-surface membrane vesicles on cultured endothelial cells. Using this approach, we observed and quantitatively measured at least two populations of cell-surface membrane vesicles, a nanoscale population (<500 nm in diameter peaking at ∼250 nm) and a microscale population (from 500 nm to ∼2 μm peaking at ∼0.8 μm), whereas confocal microscopy only detected the microscale population. The AFM-based pit-measuring method is potentially useful for studying cell-surface membrane vesicles and for investigating the mechanisms of membrane vesicle formation/release.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2017

Evaluation of Neutron Flux on the Surface of a PWR Dry Storage Cask - 17574

Since the construction of a dry storage facility for spent nuclear fuel is expected in Korea, several methods have been studied for assuring the safety of pressurized-water reactor (PWR) spent fuels in dry storage casks. Existing evaluation methods are mostly based on detection technology of gamma-rays. However, the gamma-ray detection methods have high uncertainties due to background radiation. Therefore, we developed an evaluation method for the spent nuclear fuel monitoring based on neutron detection. In this study, we evaluated neutron flux on the surface of a PWR dry storage cask using computational simulation. Neutron release rate and energy spectra from a Westinghouse (WH) 17x17 type spent fuel with 10 years cooling time were calculated using ORIGEN-ARP code. MCNP code was used to simulate geometry and material properties of the spent fuel assemblies and casks. Neutron flux after 10 years of cooling time of the spent fuels was calculated on the surface of top, side, and bottom of the casks. The metal cask and the concrete cask, called as KORAD-21 casks which newly developed by Korea Radioactive Waste Agency (KORAD), were selected for this study. As a result, for the metal cask, average neutron flux were 4.79x10{sup 2} neutrons/cm{sup 2} sec, 5.29x10{sup 2} neutrons/cm{sup 2} sec, and 1.47x10{sup 3} neutrons/cm{sup 2} sec on the surface of top, side, and bottom of the cask, respectively. For the concrete cask, average neutron flux on the surface of top, side and bottom of the casks were 5.07x10{sup 1} neutrons/cm{sup 2} sec, 1.18x10{sup 1} neutrons/cm{sup 2} sec, and 1.46x10{sup 3} neutrons/cm{sup 2} sec, respectively. The study results can be applied to evaluate characteristics of PWR spent fuels and the neutron flux of dry storage cask. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Fission Product Gas Monitoring During Fuel Drying Operations - 20094

The goal of the project was to devise and implement a method of accurately qualifying any noble gas emitted during fuel drying operations (part of the dry fuel storage process) in order to provide the data needed to validate the off-site dose calculations. The imputes of the project was the NRC publishing Information Notice 18-01, 'Noble Fission Gas Releases During Spent Fuel Cask Loading Operations' in February 2018. The information notice describes some industry events that occurred during vacuum drying operations as part of a dry fuel campaign. The solution was devised by Fort Calhoun Station staff in partnership with Mirion Technologies technical staff. The monitoring was accomplished by directing all the effluent from the fuel storage cask vacuum drying machine through a sample chamber containing a compact ISOCS characterized CZT based gamma spectrometer connected to a Mirion Data Analyst. This resulted near real-time quantification of the radionuclides of concern. (authors)

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2013

Effect of freeze-drying and self-ignition process on the microstructural and electrochemical properties of Li{sub 4}Ti{sub 5}O{sub 12}

Graphical abstract: - Highlights: • Li{sub 4}Ti{sub 5}O{sub 12} is prepared by a method involving self-ignition of a freeze-dried gel. • Addition of NH{sub 4}NO{sub 3} modifies the self-ignition propagation mode. • Well-crystallized Li{sub 4}Ti{sub 5}O{sub 12} phase is obtained after only 2 h at 800 °C. • Li{sub 4}Ti{sub 5}O{sub 12} powder has 161 mAh g{sup −1} capacity and good retention at C/4 rate. - Abstract: Crystalline Li{sub 4}Ti{sub 5}O{sub 12} is synthesized by a method involving the freeze-drying and self-ignition of a gel prepared from titanium isopropoxide, lithium nitrate and hydroxypropylmethylcellulose (HPMC). This synthesis route yields crystalline Li{sub 4}Ti{sub 5}O{sub 12} particles after calcination at 800 °C for 2 h. In an alternative route, addition of ammonium nitrate shifts the self-ignition mode from wave-like propagation to simultaneous. Powders with different microstructures are thereby obtained. Electrochemical characterization shows that the best results for Li{sup +} intercalation/desintercalation are obtained for the powder prepared without ammonium nitrate addition. These results highlight the necessity for a control of the self-ignition mode to obtain adequate properties.

36 MATERIALS SCIENCE↗