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At least 19 records

Aluminization Coatings and Glass Seals for High Temperature Systems - CRADA 536 (Final Report)

The objective of this project was to demonstrate the suitability of PNNL’s Reactive Air Aluminization (RAA) coatings (US Patent Numbers 10,577,694, 10,378,094, and 9,481,923) for use in high-temperature systems. In particular, PNNL and Utility Global undertook a collaborative effort to explore the applicability of these coatings in Utility Global’s high-temperature hydrogen reactors where they would be used to prepare the sealing surfaces of the reactor technology. Utility Global instructed PNNL regarding their needs relating to further development of glass seal technologies suitable for use in their systems. This effort entailed alkaline earth-based silicate glass development and characterization; evaluation and characterization of reliability and compatibility of the coatings with glass seals, working environments, and substrates; performance demonstrations of representative cells and intermediate cells sealed using the glass seals and/or coatings of interest; and incorporation of the aluminization coatings and glass seals into Utility Global reactors for testing.

36 MATERIALS SCIENCE↗

Aluminization Coatings and Glass Seals for High Temperature System: CRADA 536 [Abstract Only]

The proposed work will demonstrate the suitability of PNNL Reactive Air Aluminization (RAA) coatings (US Patent Numbers 10,577,694, 10,378,094, and 9,481,923) for use in high-temperature systems. In particular, the Participant and Contractor will explore applicability of these coatings in Participant’s high-temperature hydrogen reactors where they would be used to prepare the sealing surfaces of the reactor technology. Utility Global will also instruct PNNL regarding their needs relating to the further development of glass seal technologies that are suitable for use in their systems. This effort will entail alkaline earth-based silicate glass development and characterization; evaluation and characterization of reliability and compatibility of the coatings with glass seals, working environments, and substrates; performance demonstrations of representative cells and intermediate cells sealed using the glass seals and/or coatings of interest; and incorporation of the aluminization coatings and glass seals into the reactor for full-scale testing.

08 HYDROGEN↗

Crack Growth Properties of Sealing Glasses

The crack growth properties of several sealing glasses were measured using constant stress rate testing in 2% and 95% RH (relative humidity). Crack growth parameters measured in high humidity are systematically smaller (n and B) than those measured in low humidity, and velocities for dry environments are approx. 100x lower than for wet environments. The crack velocity is very sensitivity to small changes in RH at low RH. Confidence intervals on parameters that were estimated from propagation of errors were comparable to those from Monte Carlo simulation.

Salem, Jonathan A.↗

Test Method Variability in Slow Crack Growth Properties of Sealing Glasses

The crack growth properties of several sealing glasses were measured by using constant stress rate testing in ~2 and 95 percent RH (relative humidity). Crack growth parameters measured in high humidity are systematically smaller (n and B) than those measured in low humidity, and crack velocities for dry environments are ~100x lower than for wet environments. The crack velocity is very sensitive to small changes in RH at low RH. Biaxial and uniaxial stress states produced similar parameters. Confidence intervals on crack growth parameters that were estimated from propagation of errors solutions were comparable to those from Monte Carlo simulation. Use of scratch-like and indentation flaws produced similar crack growth parameters when residual stresses were considered.

Salem, J. A.↗

Solid Oxide Fuel Cell Seal Glass - BN Nanotubes Composites

Solid oxide fuel cell seal glass G18 composites reinforced with approx.4 weight percent of BN nanotubes were fabricated via hot pressing. Room temperature strength and fracture toughness of the composite were determined by four-point flexure and single edge V-notch beam methods, respectively. The strength and fracture toughness of the composite were higher by as much as 90% and 35%, respectively, than those of the glass G18. Microscopic examination of the composite fracture surfaces using SEM and TEM showed pullout of the BN nanotubes, similar in feature to fiber-reinforced ceramic matrix composites with weak interfaces. Other mechanical and physical properties of the composite will also be presented.

Bansal, Narottam P.↗

Failure analysis of the lithium battery: A study of the header deposit on the cell top and diffusion within the electrode glass seal using nuclear microanalysis and FFTIR spectroscopy

The Solid Rocket Booster Range Safety System (SRBRSS) uses a lithium/poly-carbon monofluoride primary battery as a source of electrical power. After cell fabrication and activation, some battery cells have shown self discharge. One possible source of this cell discharge has been suggested to be the formation and growth of a conducting crystallized chemical compound across the glass bead insulator, electrically shorting the glass bead to the casing. This laboratory has begun an analysis of this compound, the glass seal holding the cathode into place, and the cell electrolyte, using Fast Fourier Transform Infrared (FFTIR) Analysis, Rutherford Backscattering Spectroscopy (RBS), and Nuclear Reaction Microanalysis. Preliminary measurements have confirmed the existence of lithium, nitrogen, fluorine, and oxygen on a reddish-brown deposit covering parts of the glass seal holding the positive electrode in place. Cells using Li metal electrodes, have many advantages over conventional primary batteries. One principal disadvantage of using Li batteries on a commercial basis would be the environmental impact of the fluorocarbon material. Another would be the relatively high expense of (CF)n.

Hassan, Razi A.↗

Thermal shock testing for assuring reliability of glass-sealed microelectronic packages

Tests were performed to determine if thermal shocking is destructive to glass-to-metal seal microelectronic packages and if thermal shock step stressing can compare package reliabilities. Thermal shocking was shown to be not destructive to highly reliable glass seals. Pin-pull tests used to compare the interfacial pin glass strengths showed no differences between thermal shocked and not-thermal shocked headers. A 'critical stress resistance temperature' was not exhibited by the 14 pin Dual In-line Package (DIP) headers evaluated. Headers manufactured in cryogenic nitrogen based and exothermically generated atmospheres showed differences in as-received leak rates, residual oxide depths and pin glass interfacial strengths; these were caused by the different manufacturing methods, in particular, by the chemically etched pins used by one manufacturer. Both header types passed thermal shock tests to temperature differentials of 646 C. The sensitivity of helium leak rate measurements was improved up to 70 percent by baking headers for two hours at 200 C after thermal shocking.

Thomas, Walter B., III↗

Electrical connectors including glass seals and methods of fabrication

An electrical connector comprises an outer shell, at least one pin, and an insulating seal. The outer shell includes at least one side wall defining a cavity and having an inner surface. The outer shell is formed from electrically conductive material. The pin is positioned within the cavity and is also formed from electrically conductive material. The insulating seal is configured to provide electrical isolation of the pin and fills the cavity between the inner surface of the side wall and the pin. The insulating seal is formed from glass doped with a transition metal oxide.

Eichorst, Dennis J.↗

Crystallization Kinetics of a Solid Oxide Fuel Cell Seal Glass by Differential Thermal Analysis

Crystallization kinetics of a barium calcium aluminosilicate glass (BCAS), a sealant material for planar solid oxide fuel cells, have been investigated by differential thermal analysis (DTA). From variation of DTA peak maximum temperature with heating rate, the activation energy for glass crystallization was calculated to be 259 kJ/mol. Development of crystalline phases on thermal treatments of the glass at various temperatures has been followed by powder x-ray diffraction. Microstructure and chemical composition of the crystalline phases were investigated by scanning electron microscopy and energy dispersive spectroscopic (EDS) analysis. BaSiO3 and hexacelsian (BaAl2Si2O8) were the primary crystalline phases whereas monoclinic celsian (BaAl2Si2O8) and (Ba(x), Ca(y))SiO4 were also detected as minor phases. Needle-shaped BaSiO3 crystals are formed first, followed by the formation of other phases at longer times of heat treatments. The glass does not fully crystallize even after long term heat treatments at 750 to 900 C.

Bansal, Narottam P.↗

Measuring Humidity in Sealed Glass Encasements

A technique has been devised for measuring the relative humidity levels in the protective helium/water vapor atmosphere in which the Declaration of Independence, the United States Constitution, and the Bill of Rights are encased behind glass panels on display at the National Archives in Washington, DC. The technique is noninvasive: it does not involve penetrating the encasements (thereby risking contamination or damage to the priceless documents) to acquire samples of the atmosphere. The technique could also be applied to similar glass encasements used to protect and display important documents and other precious objects in museums. The basic principle of the technique is straightforward: An encasement is maintained at its normal display or operating temperature (e.g., room temperature) while a portion of its glass front panel is chilled (see Figure 1) until condensed water droplets become visible on the inside of the panel. The relative humidity of the enclosed atmosphere can then be determined as a known function of the dew point, the temperature below which the droplets condense. Notwithstanding the straightforwardness of the basic principle, careful attention to detail is necessary to enable accurate determination of the dew point. In the initial application, the affected portion of the glass panel was cooled by contact with an aluminum plate that was cooled by a thermoelectric module, the exhaust heat of which was dissipated by a heat sink cooled by a fan. A thermocouple was used to measure the interior temperature of the aluminum plate, and six other thermocouples were used to measure the temperatures at six locations on the cooled outer surface of the glass panel (see Figure 2). Thermal grease was applied to the aluminum plate and the thermocouples to ensure close thermal contact. Power was supplied to the thermoelectric module in small increments, based on previous laboratory tests. A small flashlight and a magnifying glass were used to look for water droplets condensing on the inner surface of the glass. The temperature readings of the thermocouples were taken during cool-down and upon observing condensation. In determining the dew point, it was necessary to make a correction for the differences between the temperatures measured on the chilled outer surface of the glass and the temperature of the inner surface, where the condensation took place. The correction was derived from a laboratory test on a measurement setup that was nearly identical, except that the dew location on the inner surface was also instrumented with a thermocouple. The test showed that the temperature at the dew location on the inner surface of the glass panel was 0.9 C above the temperature determined from the measurements on the chilled outer surface of the panel.

West, James W.↗

Experimental Ecosystems Sealed in Glass

Report describes investigation of dynamics of microbial ecosystems sealed in 1-liter flasks and exposed to Sunlight or artifical light for extended periods. Many organisms survived more than 15 years. Such systems have primary productivity and quantum efficiencies comparable to estimates for Earth's ecosystems.

Hanson, J. A.↗

High temperature storage characteristics of lithium sulfur dioxide cells

Hermetically sealed SO2 cells were developed to eliminate SO2 diffusion and its adverse effects on shelf life. A two part barrier coating material was applied to the internal surface of the glass seal and cured under a predetermined thermal profile in order to prevent the self discharge associated with glass seal corrosion.

Watson, T.↗

PRODUCTION OF GLASS-TO-METAL SEALS USING ADDITIVE MANUFACTURING TECHNIQUES

Glass-to-metal (GtM) seals are hermetic barriers between glass and metal components, often used in the electronic and vacuum industries. Creating the seals traditionally requires heating all the components to the glass melting temperature, where the glass will flow and bond to the metal. Due to the manufacturing constraints of the individual components and sealing conditions there are geometric and material restrictions. Additive manufacturing techniques were used to make GtM seals to reduce these restrictions. Hermetic, single pin seals were produced using printed metal shells, by selective laser melting (SLM), and digital light processing (DLP) printed glass preforms. Glass preforms were printed with photosensitive resin mixed with a silicate sealing glass powder in a 1:2 weight ratio. Thermal analysis, TGA/DSC, and screening experiments were used to determine an organic removal schedule. Video techniques determined a sintering schedule by producing a densification curve at different isothermal holds which were fit with a viscous sintering model. Single pin seals were also produced use a laser assisted manufacturing (LAM) process as an alternative to the conventional furnace sealing process. A Nd:YAG laser was focused on a solid glass preform, heating the glass to form the glass-metal bond. The sealing glass was doped with a transition metal oxide, Fe2O3 or CuO, to increase absorption of the laser wavelength. The interface of hermetic LAM seals were analyzed using electron microscopy, compared to conventional prepared seals, finding a reduction of interfacial morphologies.

Read, Aaron Reece↗

Reliability and Durability Testing of Glass Ceramic Seals for Praxair’s Oxygen Transport Membranes

Praxair has been developing Oxygen Transport Membrane (OTM) systems for the efficient conversion of natural gas to syngas which can subsequently be used in chemical synthesis, generation of industrial gases (H2, CO) or synthesis of liquid fuels. One of the technical barriers for commercialization of this technology is the reliability of key components of OTM systems – Seals and Membranes. Praxair has been testing these components at the process conditions expected for commercial systems. However, long-term durability data is currently limited and is not sufficiently available to make well informed predictions of OTM reliability which represents one of the major risks that could prevent the technology from being fully commercialized. Pacific Northwest National Laboratory (PNNL) has been developing high temperature seals and ceramic membranes for applications similar to OTM systems such as Solid Oxide Fuel Cells. The goal of the cooperative development between Praxair and PNNL is to generate long-term data such that there is sufficient confidence in the OTM seal and membrane reliability predictions to enable the process technology to be fully commercialized.

03 NATURAL GAS↗