Spectral mapping of zeolite bearing paleolake deposits at Lake Tecopa, California and its implications for mapping zeolites on Mars
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Gayantha R.L. Kodikara↗
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The growth of zeolites A, X and mordenite in space
Zeolites are a class of crystalline aluminosilicate materials that form the backbone of the chemical process industry worldwide. They are used primarily as adsorbents and catalysts and support to a significant extent the positive balance of trade realized by the chemical industry in the United States (around $19 billion in 1991). The magnitude of their efforts can be appreciated when one realizes that since their introduction as 'cracking catalysts' in the early 1960's, they have saved the equivalent of 60 percent of the total oil production from Alaska's North Slope. Thus the performance of zeolite catalysts can have a profound effect on the U.S. economy. It is estimated that a 1 percent increase in yield of the gasoline fraction per barrel of oil would represent a savings of 22 million barrels of crude oil per year, representing a reduction of $400 million in the United States' balance of payments. Thus any activity that results in improvement in zeolite catalyst performance is of significant scientific and industrial interest. In addition, due to their 'stability,' uniformity, and, within limits, their 'engineerable' structures, zeolites are being tested as potential adsorbents to purify gases and liquids at the parts-per-billion levels needed in today's electronic, biomedical, and biotechnology industries and for the environment. Other exotic applications, such as host materials for quantum-confined semiconductor atomic arrays, are also being investigated. Because of the importance of this class of material, extensive efforts have been made to characterize their structures and to understand their nucleation and growth mechanisms, so as to be able to custom-make zeolites for a desired application. To date, both the nucleation mechanics and chemistry (such as what are the 'key' nutrients) are, as yet, still unknown for many, if not all, systems. The problem is compounded because there is usually a 'gel' phase present that is assumed to control the degree of supersaturation, and this gel undergoes a continuous 'polymerization' type reaction during nucleation and growth. Generally, for structure characterization and diffusion studies, which are useful in evaluating zeolites for improving yield in petroleum refining as well as for many of the proposed new applications (e.g., catalytic membranes, molecular electronics, chemical sensors) large zeolites (greater than 100 to 1000 times normal size) with minimum lattice defects are desired. Presently, the lack of understanding of zeolite nucleation and growth precludes the custom design of zeolites for these or other uses. It was hypothesized that the microgravity levels achieved in an orbiting spacecraft could help to isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation, which occurs since zeolites are twice as dense as the solution from which they are formed. This was expected to promote larger crystals by allowing growing crystals a longer residence time in a high-concentration nutrient field. Thus it was hypothesized that the microgravity environment of Earth orbit would allow the growth of large, more defect-free zeolite crystals in high yield.
Sacco, Albert, Jr.↗
Growth of zeolite crystals in the microgravity environment of space
Zeolites are hydrated, crystalline aluminosilicates with alkali and alkaline earth metals substituted into cation vacancies (Equation A) M(sub 2/n) 0-Al203-XSi02-YH20 A They have a uniform internal channel system which makes them ideal for use as catalysts and adsorbents. Presently zeolite materials constitute a 1-2 mi 11 ion dol lar/year business. Typically zeolite crystals are 3-8 µm along their characteristic dimension (e.g., edge). Larger zeolite crystals are desirable. Large crystals will allow more detail characterization of their complex crystal structures. Also, they will help improve reactor performance, may be used as membrane separators, and they should enhance basic studies in molecular diffusion in zeolites. Large zeolite crystals have been produced (100-200 µm) ; however, they have taken restrictively long times to grow. It has been proposed if the rate of nucleation or in some other way the number of nuclei can be lowered, fewer, larger crystals will be formed. provide an ideal condition to achieve rapid growth of large zeolite crystals (e.g., >l00 µm). Since settling crystals are believed to cause secondary nucleation, by limiting crystal movement by suspension in the zero gravity environment, fewer crystals will form, but they will grow larger. The objective of the project is to establish if large zeolite crystals can be formed rapidly in space.
A. Sacco, Jr.↗
Zeolites on Mars: Prospects for Remote Sensing
The Martian surface composition measured by Viking can be represented by several combinations of minerals incorporating major fractions of zeolites known to occur in altered mafic rocks and polar soils on Earth. The abundant occurrence of zeolites on Mars is consistent with what is known about both the physical and chemical environment of that planet. The laboratory reflectance spectra (0.65 to 2.55 microns) of a number of relatively pure zeolite minerals and some naturally occurring zeolite-clay soils were measured. All of the spectra measured are dominated by strong absorption near 1.4 and 1.9 microns and a steep reflectance drop longward of about 2.2 microns, all of which are due to abundant H2O. Weaker water overtone bands are also apparent, and in most cases there is spectral evidence for minor Fe(3+). In these features the zeolite spectra are similar to spectra of smectite clays which have abundant interlayer water. The most diagnostic difference between clay and zeolite spectra is the total absence in the zeolites of the weak structural OH absorption.
E S Gaffney↗
Zeolite Crystal Growth (ZCG) Flight on USML-2
The extensive use of zeolites and their impact on the world's economy has resulted in many efforts to characterize their structure, and improve the knowledge base for nucleation and growth of these crystals. The zeolite crystal growth (ZCG) experiment on USML-2 aimed to enhance the understanding of nucleation and growth of zeolite crystals, while attempting to provide a means of controlling the defect concentration in microgravity. Zeolites A, X, Beta, and Silicalite were grown during the 16 day - USML-2 mission. The solutions where the nucleation event was controlled yielded larger and more uniform crystals of better morphology and purity than their terrestrial/control counterparts. The external surfaces of zeolite A, X, and Silicalite crystals grown in microgravity were smoother (lower surface roughness) than their terrestrial controls. Catalytic studies with zeolite Beta indicate that crystals grown in space exhibit a lower number of Lewis acid sites located in micropores. This suggests fewer structural defects for crystals grown in microgravity. Transmission electron micrographs (TEM) of zeolite Beta crystals also show that crystals grown in microgravity were free of line defects while terrestrial/controls had substantial defects.
Sacco, Albert, Jr.↗
Zeolite crystal growth in space
The growth of large, uniform zeolite crystals in high yield in space can have a major impact on the chemical process industry. Large zeolite crystals will be used to improve basic understanding of adsorption and catalytic mechanisms, and to make zeolite membranes. To grow large zeolites in microgravity, it is necessary to control the nucleation event and fluid motion, and to enhance nutrient transfer. Data is presented that suggests nucleation can be controlled using chemical compounds (e.g., Triethanolamine, for zeolite A), while not adversely effecting growth rate. A three-zone furnace has been designed to perform multiple syntheses concurrently. The operating range of the furnace is 295 K to 473 K. Teflon-lined autoclaves (10 ml liquid volume) have been designed to minimize contamination, reduce wall nucleation, and control mixing of pre-gel solutions on orbit. Zeolite synthesis experiments will be performed on USML-1 in 1992.
Sacco, Albert, Jr.↗
Oxygen and hydrogen isotope geochemistry of zeolites
Oxygen and hydrogen isotope ratios for natural samples of the zeolites analcime, chabazite, clinoptilolite, laumontite, mordenite, and natrolite have been obtained. The zeolite samples were classified into sedimentary, hydrothermal, and igneous groups. The ratios for each species of zeolite are reported. The results are used to discuss the origin of channel water, the role of zeolites in water-rock interaction, and the possibility that a calibrated zeolite could be used as a low-temperature geothermometer.
Karlsson, Haraldur R.↗
(Preliminary) Effects of Ball Milling Zeolite Powders for Use in Additively Manufactured Solid Sorbents
Zeolite 13X is favorable to be used as an adsorbent in carbon dioxide (CO2) removal from the spacecraft cabin air. Reducing the size of the zeolite particles and particle size distribution is thought to increase the capacity of CO2 adsorption of the zeolite 13X powder, and potentially increase its manufacturability as a paste for additive manufacturing or slip casting. This paper will go into detail on the process of using ball milling in order to reduce particle size and particle size distribution of commercial zeolite 13X powder, as well as to characterize CO2 adsorption and manufacturability of the milled powder. Both dry and wet ball milling was analyzed during the experiment. Studies were also ran on the amount of time the powder was milled, rotational speed of the milling machine, ball to powder ratio, ball to jar ratio, and ethanol to powder ratio. The processed powder was then characterized through laser diffraction, SEM, and surface measurement techniques to show that particle size and particle size distribution could be reduced, and to show the effect of the reduced particle size and particle size distribution on CO2 adsorption and manufacturability.
zeolite↗
Experiment 3: Zeolite Crystal Growth in Microgravity- The USML-2 Mission
The extensive use of zeolites and their impact on the world's economy leads to many efforts to characterize their structure, and to improve the knowledge base for nucleation and growth of these crystals. The Zeolite Crystal Growth (ZCG) experiment on USML-2 aims to enhance the understanding of nucleation and growth of zeolite crystals while attempting to provide a means of controlling the defect concentration in microgravity. Zeolites A, X, Beta, and Silicalite were grown during the 16-day USML-2 mission. The solutions where the nucleation event was controlled yielded larger and more uniform crystals of better morphology and purity than their terrestrial/control counterparts. Space-grown Beta crystals were free of line defects while terrestrial/controls had substantial defects.
Bac, Nurcan↗
Zeolites on Mars: Possible environmental indicators in soils and sediments
Weathering products should serve as indicators of weathering environments and may provide the best evidence of the nature of climate change on Mars. No direct mineralogical measurements of Martian regolith were performed by the Viking missions, but the biology and X-ray fluorescence experiments provided some information on the physiochemical properties of Martian regolith. Most post-Viking studies of candidate weathering products have emphasized phyllosilicates and Fe-oxides; zeolites are potentially important, but overlooked, candidate Martian minerals. Zeolites would be important on Mars for three different reasons. First, they are major sinks of atmospheric gases and, per unit mass, are stronger and more efficient sorbents than are phyllosilicates. Secondly, they can be virtually unique sorbents and shelters for organic compounds and possible catalysts for organic-based reactions. Finally, their exchangeable ions are good indicators of the chemical properties of solutions with which they have communicated. Accordingly, the search for information on past compositions of the Martian atmosphere and hydrosphere should find zeolites to be rich repositories.
Ming, D. W.↗
Copper-Exchanged Zeolite L Traps Oxygen
Brief series of simple chemical treatments found to enhance ability of zeolite to remove oxygen from mixture of gases. Thermally stable up to 700 degrees C and has high specific surface area which provides high capacity for adsorption of gases. To increase ability to adsorb oxygen selectively, copper added by ion exchange, and copper-exchanged zeolite reduced with hydrogen. As result, copper dispersed atomically on inner surfaces of zeolite, making it highly reactive to oxygen, even at room temperature. Reactivity to oxygen even greater at higher temperatures.
Sharma, Pramod K.↗
Zeolite crystal growth in space - What has been learned
Three zeolite crystal growth experiments developed at WPI have been performed in space in last twelve months. One experiment, GAS-1, illustrated that to grow large, crystallographically uniform crystals in space, the precursor solutions should be mixed in microgravity. Another experiment evaluated the optimum mixing protocol for solutions that chemically interact ('gel') on contact. These results were utilized in setting the protocol for mixing nineteen zeolite solutions that were then processed and yielded zeolites A, X and mordenite. All solutions in which the nucleation event was influenced produced larger, more 'uniform' crystals than did identical solutions processed on earth.
Sacco, A., Jr.↗
Large zeolites - Why and how to grow in space
The growth of zeolite crystals which are considered to be the most valuable catalytic and adsorbent materials of the chemical processing industry are discussed. It is proposed to use triethanolamine as a nucleation control agent to control the time release of Al in a zeolite A solution and to increase the average and maximum crystal size by 25-50 times. Large zeolites could be utilized to make membranes for reactors/separators which will substantially increase their efficiency.
Sacco, Albert, Jr.↗
Modeling of Macroscopic/Microscopic Transport and Growth Phenomena in Zeolite Crystal Solutions Under Microgravity Conditions
Crystals grown from liquid solutions have important industrial applications. Zeolites, for instance, a class of crystalline aluminosilicate materials, form the backbone of the chemical process industry worldwide, as they are used as adsorbents and catalysts. Many of the phenomena associated with crystal growth processes are not well understood due to complex microscopic and macroscopic interactions. Microgravity could help elucidate these phenomena and allow the control of defect locations, concentration, as well as size of crystals. Microgravity in an orbiting spacecraft could help isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation. In addition, crystals will stay essentially suspended in the nutrient pool under a diffusion-limited growth condition. This is expected to promote larger crystals by allowing a longer residence time in a high-concentration nutrient field. Among other factors, the crystal size distribution depends on the nucleation rate and crystallization. These two are also related to the "gel" polymerization/depolymerization rate. Macroscopic bulk mass and flow transport and especially gravity, force the crystals down to the bottom of the reactor, thus forming a sedimentation layer. In this layer, the growth rate of the crystals slows down as crystals compete for a limited amount of nutrients. The macroscopic transport phenomena under certain conditions can, however, enhance the nutrient supply and therefore, accelerate crystal growth. Several zeolite experiments have been performed in space with mixed results. The results from our laboratory have indicated an enhancement in size of 30 to 70 percent compared to the best ground based controls, and a reduction of lattice defects in many of the space grown crystals. Such experiments are difficult to interpret, and cannot be easily used to derive empirical or other laws since many physical parameters are simultaneously involved in the process. At the same time, however, there is increased urgency to develop such an understanding in order to more accurately quantify the process. In order to better understand the results obtained from our prior space experiments, and design future experiments, a detailed fluid dynamic model simulating the crystal growth mechanism is required. This will not only add to the fundamental knowledge on the crystallization of zeolites, but also be useful in predicting the limits of size and growth of these important industrial materials. Our objective is to develop macro/microscopic theoretical and computational models to study the effect of transport phenomena in the growth of crystals grown in solutions. Our effort has concentrated so far in the development of separate macroscopic and microscopic models. The major highlights of our accomplishments are described.
Gatsonis, Nikos A.↗
Hydrogen Purification Using Natural Zeolite Membranes
The School of Science at Universidad del Turabo (UT) have a long-lasting investigation plan to study the hydrogen cleaning and purification technologies. We proposed a research project for the synthesis, phase analysis and porosity characterization of zeolite based ceramic perm-selective membranes for hydrogen cleaning to support NASA's commitment to achieving a broad-based research capability focusing on aerospace-related issues. The present study will focus on technology transfer by utilizing inorganic membranes for production of ultra-clean hydrogen for application in combustion. We tested three different natural zeolite membranes (different particle size at different temperatures and time of exposure). Our results show that the membranes exposured at 900 C for 1Hr has the most higher permeation capacity, indicated that our zeolite membranes has the capacity to permeate hydrogen.
DelValle, William↗
Co-Adsorption of Carbon Dioxide on Zeolite 13X in the Presence of Preloaded Water
Environmental Control and Life Support requires highly effective CO2 removal systems. The current system onboard the International Space Station is known as Carbon Dioxide Removal Assembly. Recent high-fidelity simulation of this system predicted a major efficiency gain via reduction of desiccant zeolite. Commercial beaded 13X zeolite is used in the desiccant bed to scrub water below 1 ppm but is also a highly active CO2 sorbent. The simultaneous adsorption of water vapor and CO2 is known to strongly favor water, but more accurate measurements are needed. This work details the characterization of the zeolite to be used in the next-generation CO2 removal system for co-adsorption of water and CO2.
Cmarik, Gregory E↗
Preliminary market analysis for large zeolite crystals
Zeolite crystals are used in the manufacture of countless products today, which utilize their properties of absorption, ion exchange, and catalysis. It was determined that zeolites grown in space could be much larger in size than any of those currently available on Earth. The objective was to identify and examine some of the potential uses for these larger crystals. Of the several industries examined, the medical and nuclear industries offer the greatest potential.
Doblmaier, Thomas↗
Regenerative Cu/La zeolite supported desulfurizing sorbents
Efficient, regenerable sorbents for removal of H2S from fluid hydrocarbons such as diesel fuel at moderate condition comprise a porous, high surface area aluminosilicate support, suitably a synthetic zeolite, and most preferably a zeolite having a free lattice opening of at least 6 Angstroms containing from 0.1 to 0.5 moles of copper ions, lanthanum ions or their mixtures. The sorbent removes sulfur from the hydrocarbon fuel in high efficiency and can be repetitively regenerated without loss of activity.
Voecks, Gerald E.↗