Formation of Residual Gases from Source Materials in Closed Crystal Growth Systems

NASA Technical Reports Server (NTRS)

Palosz, W.; Rose, M. Franklin (Technical Monitor)

2001-01-01

Different, non-constituent cases are present in crystal growth systems and may affect processes like growth rate in PVT or voids formation and detached solidification in melt growth systems. The presence of the gas may be detrimental or advantageous depending on its amount and composition, and on the process in question. The presence of the cases, their amount and composition, can be caused and changed by diffusion through and desorption from the growth container material. We have investigated these phenomena for silica glass ampoules. We also found, that residual cases can be generated by the source materials: even very high purity commercial elements and compounds may contain trace amounts of impurities, particularly oxides. The oxides may have low volatilities themselves but their reaction with other species, particularly carbon and hydrogen, may produce volatile compounds like water or carbon oxides. The amount of the gas and its composition is dependent on the original purity of the material (oxide contaminants) and the heat treatment of the source prior to sealing. In many cases. particularly at temperatures below about 900 C and in well-outgassed ampoules, this mechanism dominates. The problem is of a particular importance in sealed systems where the amount and composition of the gas cannot be directly controlled. Therefore, a reasonable knowledge and understanding of the origin, composition, magnitude, and change with time of gases present in sealed ampoules may be important for a meaningful control and interpretation of crystal growth processes. We have investigated this phenomenon in more details for a number of elements and compounds, primarily for II-VI and IV-VI materials. Different source pre-treatment and annealing procedures were applied, and subsequent consecutive annealings and measurements were done to determine the origin and development of the gas in the systems.

Foamed Bulk Metallic Glass (Foam) Investigation

NASA Technical Reports Server (NTRS)

2004-01-01

This soldering iron has an evacuated copper capsule at the tip that contains a pellet of Bulk Metallic Glass (BMG) aboard the International Space Station (ISS). Prior to flight, researchers sealed a pellet of bulk metallic glass mixed with microscopic gas-generating particles into the copper ampoule under vacuum. Once heated in space, such as in this photograph, the particles generated gas and the BMG becomes a viscous liquid. The released gas made the sample foam within the capsule where each microscopic particle formed a gas-filled pore within the foam. The inset image shows the oxidation of the sample after several minutes of applying heat. Although hidden within the brass sleeve, the sample retained the foam shape when cooled, because the viscosity increased during cooling until it was solid.

Glass-Ampoule Breaker

NASA Technical Reports Server (NTRS)

Christianson, R. C.; Kaushik, Surender M.; Davis, Dennis D.

1995-01-01

Device breaks glass ampoule in repeatable manner and retains gaseous content so pressure of gas measured accurately. In addition, protects technician from gaseous contents, which can be hazardous. Broken glass and sample materials easily removed for disposal or analysis. Apparatus developed for use in experiments on compatibility of materials.

Solidification Using the Baffle in Sealed Ampoules

NASA Technical Reports Server (NTRS)

Ostrogorsky, A.; Marin, C.; Churilov, A.; Volz, M. P.; Bonner, W. A.; Spivey, R. A.; Smith, G.

2003-01-01

Solidification Using a Baffle in Sealed Ampoules (SUBSA) is the first investigation conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. In July, August and September of 2002, 8 single crystals of InSb, doped with Te and Zn, were directionally solidified in microgravity. Ground based tests, related numerical modeling and images of the growth process obtained in microgravity are presented.

Biscayne aquifer drinking water (USGS45): a new isotopic reference material for δ2H and δ18O measurements of water

USGS Publications Warehouse

Lorenz, Jennifer M.; Tarbox, Lauren V.; Buck, Bryan; Qi, Haiping; Coplen, Tyler B.

2014-01-01

RATIONALE As a result of the scarcity of isotopic reference waters for daily use, a new secondary isotopic reference material for international distribution has been prepared from drinking water collected from the Biscayne aquifer in Ft. Lauderdale, Florida. METHODS This isotopic reference water was filtered, homogenized, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity, and measured by dual-inlet isotope-ratio mass spectrometry. This reference material is available by the case of 144 glass ampoules containing either 4 mL or 5 mL of water in each ampoule. RESULTS The δ2H and δ18O values of this reference material are –10.3 ± 0.4 ‰ and –2.238 ± 0.011 ‰, respectively, relative to VSMOW, on scales normalized such that the δ2H and δ18O values of SLAP reference water are, respectively, –428 and –55.5 ‰. Each uncertainty is an estimated expanded uncertainty (U = 2uc) about the reference value that provides an interval that has about a 95 % probability of encompassing the true value. CONCLUSIONS This isotopic reference material, designated as USGS45, is intended as one of two isotopic reference waters for daily normalization of stable hydrogen and oxygen isotopic analysis of water with an isotope-ratio mass spectrometer or a laser absorption spectrometer. 

Redox-dependent solubility of technetium in low activity waste glass

NASA Astrophysics Data System (ADS)

Soderquist, Chuck Z.; Schweiger, Michael J.; Kim, Dong-Sang; Lukens, Wayne W.; McCloy, John S.

2014-06-01

The solubility of technetium was measured in a Hanford low activity waste (LAW) glass simulant, to investigate the extent that technetium solubility controls the incorporation of technetium into LAW glass. A series of LAW glass samples, spiked with 500-6000 ppm of Tc as potassium pertechnetate, were melted at 1000 °C in sealed fused quartz ampoules. Technetium solubility was determined in the quenched bulk glass to be 2000-2800 ppm, with slightly reducing conditions due to choice of milling media resulting in reductant contamination and higher solubility. The chemical form of technetium obtained by X-ray absorption near edge spectroscopy is mainly isolated, octahedrally-coordinated Tc(IV), with a minority of Tc(VII) in some glasses and TcO2 in two glasses. The concentration and speciation of technetium depends on glass redox and amount of technetium added. Salts formed at the top of higher technetium loaded glasses during the melt. The results of this study show that technetium solubility should not be a factor in technetium retention during melting of Hanford LAW glass.

Material Science

NASA Image and Video Library

2004-07-12

This soldering iron has an evacuated copper capsule at the tip that contains a pellet of Bulk Metallic Glass (BMG) aboard the International Space Station (ISS). Prior to flight, researchers sealed a pellet of bulk metallic glass mixed with microscopic gas-generating particles into the copper ampoule under vacuum. Once heated in space, such as in this photograph, the particles generated gas and the BMG becomes a viscous liquid. The released gas made the sample foam within the capsule where each microscopic particle formed a gas-filled pore within the foam. The inset image shows the oxidation of the sample after several minutes of applying heat. Although hidden within the brass sleeve, the sample retained the foam shape when cooled, because the viscosity increased during cooling until it was solid.

Residual Gas in Closed Systems. III: Development and Reduction of Gases Generated by Source Materials

NASA Technical Reports Server (NTRS)

Palosz, W.

2003-01-01

The amounts and composition of residual gases formed in sealed ampoules loaded with different sources (elements and II-VI and IV-VI compounds) after consecutive annealings were investigated. A given source was subjected to a series of heat treatments, with intermediate measurements and removal of the gas accumulated in the system. The results of these experiments are discussed in terms of the underlying thermochemical and kinetic phenomena and practical limitations of reducing the amount of residual gases in sealed ampoules.

Influence of the glass packing on the contamination of pharmaceutical products by aluminium. Part III: Interaction container-chemicals during the heating for sterilisation.

PubMed

Bohrer, Denise; do Nascimento, Paulo Cícero; Binotto, Regina; Becker, Emilene

2003-01-01

The interaction of chemicals with the container materials during heating for sterilisation was investigated, storing the components of parenteral nutrition solutions individually in sealed glass ampoules and in contact with a rubber stopper, and heating the system at 121 degrees C for 30 min. Subsequently, the aluminium content of the solutions was measured by atomic absorption spectrometry (AAS). The assay was also carried out with acids, alkalis and some complexing agents for Al. The containers were decomposed and also assayed for aluminium. 30 different commercial solutions for parenteral nutrition, stored either in glass or in plastic containers, were assayed measuring the aluminium present in the solutions and in the container materials. The results of all investigated container materials revealed an aluminium content of 1.57% Al in glass, 0.05% in plastic and 4.54% in rubber. The sterilisation procedure showed that even pure water was able to extract Al from glass and rubber, 22.5 +/- 13.3 microg/L and 79.4 +/- 22.7 microg/L respectively, while from plastic the aluminium leached was insignificant. The Al released from glass ampoules laid between 20 microg/L for leucine, ornithine and lysine solutions and 1500 microg/L for solutions of basic phosphates and bicarbonate; from rubber stoppers it reached levels over 500 microg/L for cysteine, aspartic acid, glutamic acid and cystine solutions. Ion-exchange properties and influence of pH can explain the interaction of glass with some chemicals (salts, acids and alkalis), but only an affinity for aluminium could explain the action of some amino acids and other chemicals, as albumin and heparin, on glass and rubber, considering the aluminium release. Experiments with complexing agents for Al allowed to conclude that the higher the stability constant of the complex, the higher the Al release from the container material.

Growth of CdZnTe Crystals the Bridgman Technique with Controlled Overpressures of Cd

NASA Technical Reports Server (NTRS)

Su, Ching-Hu; Lehoczky, S. L.

2008-01-01

Cd(1-x)Zn(x)Te crystals with x = 0.15 and 0.20, were grown in this study by closed-ampoule directional solidification (Bridgman) technique with a controlled Cd overpressure. The growth ampoule was made of quartz with inner diameter from 20 to 40 mm and a tapered length of 2.5 cm at the growth tip. Both unseeded and seeded growths were performed with total material charges up to 400 g. After the loading of starting CdZnTe material, a typical amount of 2 g of Cd was also loaded inside a Cd reservoir basket, which was attached beneath the seal-off cup. The ampoule was sealed off under a vacuum below lxl0(exp -5) Torr. The sealed ampoule was placed inside a 4-zone Bridgman furnace - a Cd reservoir zone with a heat-pipe furnace liner on the top, followed by a hot zone, a booster heating zone and a cold zone at the bottom. The Cd zone was typically 300 to 400 C below the hot zone setting. High resistivity material has been obtained without any intentional dopants but has been reproducibly obtained with In doping. The crystalline and the electrical properties of the crystals will be reported.

Biscayne aquifer drinking water (USGS45): a new isotopic reference material for δ2H and δ18O measurements of water.

PubMed

Lorenz, Jennifer M; Tarbox, Lauren; Buck, Bryan; Qi, Haiping; Coplen, Tyler B

2014-10-15

As a result of the scarcity of isotopic reference waters for daily use, a new secondary isotopic reference material for international distribution has been prepared from drinking water collected from the Biscayne aquifer in Ft. Lauderdale, Florida. This isotopic reference water was filtered, homogenized, loaded into glass ampoules, sealed with a torch, autoclaved to eliminate biological activity, and measured by dual-inlet isotope-ratio mass spectrometry. This reference material is available by the case of 144 glass ampoules containing either 4 mL or 5 mL of water in each ampoule. The δ(2)H and δ(18)O values of this reference material are -10.3 ± 0.4‰ and -2.238 ± 0.011‰, respectively, relative to VSMOW, on scales normalized such that the δ(2)H and δ(18)O values of SLAP reference water are, respectively, -428 and -55.5‰. Each uncertainty is an estimated expanded uncertainty (U = 2uc ) about the reference value that provides an interval that has about a 95% probability of encompassing the true value. This isotopic reference material, designated as USGS45, is intended as one of two isotopic reference waters for daily normalization of stable hydrogen and oxygen isotopic analysis of water with an isotope-ratio mass spectrometer or a laser absorption spectrometer. Published in 2014. This article is a U.S. Government work and is in the public domain in the USA. Published in 2014. This article is a U.S. Government work and is in the public domain in the USA.

Combined sample collection and gas extraction for the measurement of helium isotopes and neon in natural waters

NASA Astrophysics Data System (ADS)

Roether, Wolfgang; Vogt, Martin; Vogel, Sandra; Sültenfuß, Jürgen

2013-06-01

We present a new method to obtain samples for the measurement of helium isotopes and neon in water, to replace the classical sampling procedure using clamped-off Cu tubing containers that we have been using so far. The new method saves the gas extraction step prior to admission to the mass spectrometer, which the classical method requires. Water is drawn into evacuated glass ampoules with subsequent flame sealing. Approximately 50% headspace is left, from which admission into the mass spectrometer occurs without further treatment. Extensive testing has shown that, with due care and with small corrections applied, the samples represent the gas concentrations in the water within ±0.07% (95% confidence level; ±0.05% with special handling). Fast evacuation is achieved by pumping on a small charge of water placed in the ampoule. The new method was successfully tested at sea in comparison with Cu-tubing sampling. We found that the ampoule samples were superior in data precision and that a lower percentage of samples were lost prior to measurement. Further measurements revealed agreement between the two methods in helium, 3He and neon within ±0.1%. The new method facilitates the dealing with large sample sets and minimizes the delay between sampling and measurement. The method is applicable also for gases other than helium and neon.

Reaction pathway mechanism of thermally induced isomerization of 9,12-linoleic acid triacylglycerol.

PubMed

Guo, Qin; Jiang, Fan; Deng, Zhaoxuan; Li, Qingpeng; Jin, Jing; Ha, Yiming; Wang, Feng

2017-04-01

To clarify the formation mechanism of trans linoleic acid isomers in edible oils during the heating process, trilinolein and trilinoelaidin, as representative oils, were placed in glass ampoules and sealed before heating at 180, 240 and 320 °C. The glass ampoules were removed at regular time intervals, and the contents were analyzed by infrared spectroscopy. The samples were then subjected to derivatization into their methyl esters for gas chromatographic analysis. Analysis results show that 9c,12c and 9t,12t fatty acids from trilinolein and trilinoelaidin molecules undergo chemical bond rotation, migration and degradation, leading to the formation of non-conjugated linoleic acids (NLAs), conjugated linoleic acids (CLAs) and aldehydes. The formation rate of isomers from the 9c,12c fatty acid is higher than that of the 9t,12t fatty acid. The production of aldehydes increases with heating temperature and time. The isomerization pathways involved in the formation of NLAs and CLAs during heating are clearly presented. These findings suggest possible pathways of NFA and CFA formation from heated trilinolein and trilinoelaidin, complement the mechanistic studies previously published in the literature, and provide a theoretical basis for future control of the quality and safety of fats and oils. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Thermal Stability of Otto Fuel Prepolymer

NASA Technical Reports Server (NTRS)

Tompa, Albert S.; Sandagger, Karrie H.; Bryant, William F., Jr.; McConnell, William T.; Lacot, Fernando; Carr, Walter A.

2000-01-01

Otto Fuel II contains a nitrate ester, plasticizer, and 2-NDPA as a stabilizer. Otto Fuel with stabilizers from three vendors was investigated by dynamic and isothermal DSC using samples sealed in a glass ampoule and by Isothermal Microcalorimetry (IMC) using 10 gram samples aged at 75 C for 35 days. DSC kinetics did not show differences between the stabilizer; the samples had an activation energy of 36.7 +/- 0.6 kcal/mol. However, IMC analysis was sensitive enough to detect small differences between the stabilizer, namely energy of interaction values of 7 to 14 Joules. DSC controlled cooling and heating at 5 C/min from 30 to -60 to 40 C experiments were similar and showed a crystallization peak at -48 +/- 1 C during cooling, and upon heating there was a glass transition temperature step at approx. -54 +/- 0.5 C and a melting peak at -28 +/- 0.4 C.

Thermal Stability of Otto Fuel Prepolymer

NASA Technical Reports Server (NTRS)

Tompa, Albert S.; Sandagger, Karrie H.; Bryant, William F., Jr.; McConnell, William T.; Lacot, Fernando; Carr, Walter A.

2000-01-01

Otto Fuel II contains a nitrate ester, plasticizer, and 2-NPDA as a stabilizer. Otto Fuel with stabilizers from three vendors was investigated by dynamic and isothermal differential scanning calorimetry (DSC) using samples sealed in a glass ampoule and by Isothermal Microcalorimetry (IMC) using 10 gram samples aged at 75 C for 35 days. DSC kinetics did not show differences between the stabilizer; the samples had an activation energy of 36.7 +/- 0.6 kcal/mol. However, IMC analysis was sensitive enough to detect small differences between the stabilizer, namely energy of interaction values of 7 to 14 Joules. DSC controlled cooling and heating at 5 C/min from 30 to -60 to 40 C experiments were similar and showed a crystallization peak at -48 +/- 1 C during cooling, and upon heating there was a glass transition temperature step at approx. -54 +/- 0.5 C and a melting peak at -28 +/- 0.4 C.

Diffusive Gas Loss from Silica Glass Ampoules at Elevated Temperatures

NASA Technical Reports Server (NTRS)

Palosz, W.

1998-01-01

Changes in the pressure of hydrogen, helium and neon due to diffusion through the wall of silica crystal growth ampoules at elevated temperatures were determined experimentally. We show that, while both He- and Ne-losses closely follow conventional model of diffusive gas permeation through the wall, hydrogen losses, in particular at low fill pressures, can be much larger. This is interpreted in terms of the high solubility of hydrogen in silica glasses.

Solidification Using a Baffle in Sealed Ampoules (SUBSA)

NASA Technical Reports Server (NTRS)

Marin, C.; Ostrogorsky, A. G.; Volz, M.; Luz, P.; Jeter, L.; Spivey, R.; Burton, H.; Smith, G.; Knowles, T. R.; Bonner, W. A.

2003-01-01

Solidification Using a Baffle in Sealed Ampoules (SUBSA) will be the first materials science experiment conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. The launch is schedule for May 31, 2002. Using the specially developed furnace, 10 Te and Zn-doped single crystals of InSb will be directionally solidified in microgravity. A key goal of the SUBSA investigation is to (i) clarify the origin of the melt motion in space laboratories and (ii) to reduce the magnitude of the melt motion to the point that it does not interfere with the transport phenomena. These goals will be accomplished through a special ampoule and furnace design. A disk-shaped baffle, positioned close to the freezing front, is used to reduce melt motion. Furthermore, the solidification will be visualized by using a transparent furnace, with a video camera, continuously sending images to the earth. This allows detection of bubbles and melt de-wetting that could cause surface tension driven convection. In preparation for the space experiments, 30 ground-based experiments were conducted. The results of ground based tests and numerical modeling will be presented. Based on numerical modeling, 12 mm 1D silica ampoules were selected. The small diameter ampoule favors closer placement of the baffle to the interface, without excessive radial segregation caused by forced convection while providing more damping of natural convection. The parts in the silica ampoule include 2 carbon springs made by Energy Science Laboratories, Inc., a pyrocarbon-coated graphite cylinder, pyrocarbon-coated graphite a baffle with the shaft and the InSb charge with the seed crystal grown by W.A. Bonner of Crystallod Inc.

Combined distillation and normal freezing to purify elements of groups II and VI

NASA Technical Reports Server (NTRS)

Holland, L. R.

1984-01-01

A practical system and its application to the purification of Te and Cd is described. Single crystals are grown directly in vitreous silica ampoules subsequently used for sealed Bridgman growth of (Hg-Cd)Te. The system also prepares the ampoules by heating in high vacuum. Purification of the elements is by the combined effect of distillation and normal freezing. Transport and segregation are discussed.

Material Science

NASA Image and Video Library

2003-01-22

One of the first materials science experiments on the International Space Station -- the Solidification Using a Baffle in Sealed Ampoules (SUBSA) -- will be conducted during Expedition Five inside the Microgravity Science Glovebox. The glovebox is the first dedicated facility delivered to the Station for microgravity physical science research, and this experiment will be the first one operated inside the glovebox. The glovebox's sealed work environment makes it an ideal place for the furnace that will be used to melt semiconductor crystals. Astronauts can change out samples and manipulate the experiment by inserting their hands into a pair of gloves that reach inside the sealed box. Dr. Aleksandar Ostrogorsky, a materials scientist from the Rensselaer Polytechnic Institute, Troy, N.Y., and the principal investigator for the SUBSA experiment, uses the gloves to examine an ampoule like the ones used for his experiment inside the glovebox's work area. The Microgravity Science Glovebox and the SUBSA experiment are managed by NASA's Marshall Space Flight Center in Huntsville, Ala.

Viscosity Measurement for Tellurium Melt

NASA Technical Reports Server (NTRS)

Lin, Bochuan; Li, Chao; Ban, Heng; Scripa, Rosalia N.; Su, Ching-Hua; Lehoczky, Sandor L.

2006-01-01

The viscosity of high temperature Te melt was measured using a new technique in which a rotating magnetic field was applied to the melt sealed in a suspended ampoule, and the torque exerted by rotating melt flow on the ampoule wall was measured. Governing equations for the coupled melt flow and ampoule torsional oscillation were solved, and the viscosity was extracted from the experimental data by numerical fitting. The computational result showed good agreement with experimental data. The melt velocity transient initiated by the rotating magnetic field reached a stable condition quickly, allowing the viscosity and electrical conductivity of the melt to be determined in a short period.

Gas ampoule-syringe

DOEpatents

Gay, Don D.

1986-01-01

A gas ampoule for the shipment and delivery of radioactive gases. The gas ampoule having a glass tube with serum bottle stopper on one end and a plunger tip in the opposite end all fitting in a larger plastic tube threaded on each end with absorbent between the tubes, is seated onto the internal needle assembly via a bushing associated with the plunger and locked into the syringe barrel via barrel-bushing locking caps. The design practically eliminates the possibility of personnel contamination due to an inadvertent exposure of such personnel to the contained radioactive gas.

Gas ampoule-syringe

DOEpatents

Gay, D.D.

1985-02-02

A gas ampoule for the shipment and delivery of radioactive gases. The gas ampoule having a glass tube with serum bottle stopper on one and a plunger tip in the opposite end all fitting in a larger plastic tube threaded on each end with absorbent between the tubes, is seated onto the internal needle assembly via a bushing associated with the plunger and locked into the syringe barrel via barrel-bushing locking caps. The design practically eliminates the possibility of personnel contamination due to an inadvertent exposure of such personnel to the contained radioactive gas.

Influence of Contact Angle, Growth Angle and Melt Surface Tension on Detached Solidification of InSb

NASA Technical Reports Server (NTRS)

Wang, Yazhen; Regel, Liya L.; Wilcox, William R.

2000-01-01

We extended the previous analysis of detached solidification of InSb based on the moving meniscus model. We found that for steady detached solidification to occur in a sealed ampoule in zero gravity, it is necessary for the growth angle to exceed a critical value, the contact angle for the melt on the ampoule wall to exceed a critical value, and the melt-gas surface tension to be below a critical value. These critical values would depend on the material properties and the growth parameters. For the conditions examined here, the sum of the growth angle and the contact angle must exceed approximately 130, which is significantly less than required if both ends of the ampoule are open.

Vapor crystal growth technology development: Application to cadmium telluride

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Banish, Michael; Duval, Walter M. B.

1991-01-01

Growth of bulk crystals by physical vapor transport was developed and applied to cadmium telluride. The technology makes use of effusive ampoules, in which part of the vapor contents escapes to a vacuum shroud through defined leaks during the growth process. This approach has the advantage over traditional sealed ampoule techniques that impurity vapors and excess vapor constituents are continuously removed from the vicinity of the growing crystal. Thus, growth rates are obtained routinely at magnitudes that are rather difficult to achieve in closed ampoules. Other advantages of this effusive ampoule physical vapor transport (EAPVT) technique include the predetermination of transport rates based on simple fluid dynamics and engineering considerations, and the growth of the crystal from close to congruent vapors, which largely alleviates the compositional nonuniformities resulting from buoyancy driven convective transport. After concisely reviewing earlier work on improving transport rates, nucleation control, and minimization of crystal wall interactions in vapor crystal growth, a detail account is given of the largely computer controlled EAPVT experimentation.

Response surface methodology (RSM) to evaluate moisture effects on corn stover in recovering xylose by DEO hydrolysis

Treesearch

Rita C.L.B. Rodrigues; William R. Kenealy; Diane Dietrich; Thomas W. Jeffries

2012-01-01

Response surface methodology (RSM), based on a 22 full factorial design, evaluated the moisture effects in recovering xylose by diethyloxalate (DEO) hydrolysis. Experiments were carried out in laboratory reactors (10 mL glass ampoules) containing corn stover (0.5 g) properly ground. The ampoules were kept at 160 °C for 90 min. Both DEO...

Rhenium Solubility in Borosilicate Nuclear Waste Glass: Implications for the Processing and Immobilization of Technetium-99

DOE Office of Scientific and Technical Information (OSTI.GOV)

McCloy, John S.; Riley, Brian J.; Goel, Ashutosh

2012-10-26

The immobilization of 99Tc in a suitable host matrix has proved to be an arduous task for the researchers in nuclear waste community around the world. At the Hanford site in Washington State, the total amount of 99Tc in low-activity waste (LAW) is ~1300 kg and the current strategy is to immobilize the 99Tc in borosilicate glass with vitrification. In this context, the present article reports on the solubility/retention of rhenium, a nonradioactive surrogate for 99Tc, in a LAW borosilicate glass. Due to the radioactive nature of technetium, rhenium was chosen as a simulant because of the similarity between theirmore » ionic radii and other chemical aspects. The glasses containing Re (0 – 10,000 ppm by mass) were synthesized in vacuum-sealed quartz ampoules in order to minimize the loss of Re by volatilization during melting at 1000 °C. The rhenium was found to predominantly exist as Re (VII) in all the glasses as observed by X-ray absorption near-edge structure (XANES). The solubility of Re in borosilicate glasses was determined to be ~3000 ppm (by mass) with inductively coupled plasma-optical emission spectroscopy (ICP-OES). At higher rhenium concentrations, some additional material was retained in the glasses in the form of crystalline inclusions that were detected by X-ray diffraction (XRD) and laser ablation-ICP mass spectrometry (LA-ICP-MS). The implications of these results on the immobilization of 99Tc from radioactive wastes in borosilicate glasses have been discussed.« less

RHENIUM SOLUBILITY IN BOROSILICATE NUCLEAR WASTE GLASS IMPLICATIONS FOR THE PROCESSING AND IMMOBILIZATION OF TECHNETIUM-99 (AND SUPPORTING INFORMATION WITH GRAPHICAL ABSTRACT)

DOE Office of Scientific and Technical Information (OSTI.GOV)

AA KRUGER; A GOEL; CP RODRIGUEZ

2012-08-13

The immobilization of 99Tc in a suitable host matrix has proved a challenging task for researchers in the nuclear waste community around the world. At the Hanford site in Washington State in the U.S., the total amount of 99Tc in low-activity waste (LAW) is {approx} 1,300 kg and the current strategy is to immobilize the 99Tc in borosilicate glass with vitrification. In this context, the present article reports on the solubility and retention of rhenium, a nonradioactive surrogate for 99Tc, in a LAW sodium borosilicate glass. Due to the radioactive nature of technetium, rhenium was chosen as a simulant becausemore » of previously established similarities in ionic radii and other chemical aspects. The glasses containing target Re concentrations varying from 0 to10,000 ppm by mass were synthesized in vacuum-sealed quartz ampoules to minimize the loss of Re by volatilization during melting at 1000 DC. The rhenium was found to be present predominantly as Re7 + in all the glasses as observed by X-ray absorption near-edge structure (XANES). The solubility of Re in borosilicate glasses was determined to be {approx}3,000 ppm (by mass) using inductively coupled plasma-optical emission spectroscopy (ICP-OES). At higher rhenium concentrations, some additional material was retained in the glasses in the form of alkali perrhenate crystalline inclusions detected by X-ray diffraction (XRD) and laser ablation-ICP mass spectrometry (LA-ICP-MS). Assuming justifiably substantial similarities between Re7 + and Tc 7+ behavior in this glass system, these results implied that the processing and immobilization of 99Tc from radioactive wastes should not be limited by the solubility of 99Tc in borosilicate LAW glasses.« less

Adrenaline in cardiac arrest: Prefilled syringes are faster.

PubMed

Helm, Claire; Gillett, Mark

2015-08-01

Standard ampoules and prefilled syringes of adrenaline are widely available in Australasian EDs for use in cardiac arrest. We hypothesise that prefilled syringes can be administered more rapidly and accurately when compared with the two available standard ampoules. This is a triple arm superiority study comparing the time to i.v. administration and accuracy of dosing of three currently available preparations of adrenaline. In their standard packaging, prefilled syringes were on average more than 12 s faster to administer than the 1 mL 1:1000 ampoules and more than 16 s faster than the 10 mL 1:10,000 ampoules (P < 0.01 in both comparisons). With packaging removed, the time to administration was equal for the 1 mL (1:1000) ampoule and the prefilled syringe. Accuracy of dosing was excellent with both the 10 mL (1:10 000) ampoules and prefilled syringes. The 1 mL (1:1000) ampoules delivered a small number of markedly inaccurate doses, but these did not reach statistical significance. The speed of administration of adrenaline utilising a Minijet (CSL Limited, Parkville, Victoria, Australia) is faster than using adrenaline in glass ampoules presented in their plastic packaging. Removing the plastic packaging from the 1 mL (1 mg) ampoule might result in more rapid administration similar to the Minijet. Resuscitation personnel requiring rapid access to adrenaline should consider storing it as either Minijets or ampoules devoid of packaging. These results might be extrapolatable to other clinical scenarios, including pre-hospital and anaesthesia, where other drugs are required for rapid use. © 2015 Australasian College for Emergency Medicine and Australasian Society for Emergency Medicine.

Solid oxide fuel cell having a glass composite seal

DOEpatents

De Rose, Anthony J.; Mukerjee, Subhasish; Haltiner, Jr., Karl Jacob

2013-04-16

A solid oxide fuel cell stack having a plurality of cassettes and a glass composite seal disposed between the sealing surfaces of adjacent cassettes, thereby joining the cassettes and providing a hermetic seal therebetween. The glass composite seal includes an alkaline earth aluminosilicate (AEAS) glass disposed about a viscous glass such that the AEAS glass retains the viscous glass in a predetermined position between the first and second sealing surfaces. The AEAS glass provides geometric stability to the glass composite seal to maintain the proper distance between the adjacent cassettes while the viscous glass provides for a compliant and self-healing seal. The glass composite seal may include fibers, powders, and/or beads of zirconium oxide, aluminum oxide, yttria-stabilized zirconia (YSZ), or mixtures thereof, to enhance the desirable properties of the glass composite seal.

Interface Shape and Convection During Solidification and Melting of Succinonitrile

NASA Technical Reports Server (NTRS)

Degroh, Henry C., III; Lindstrom, Tiffany

1994-01-01

An experimental study was conducted of the crystal growth of succinonitrile during solidification, melting, and no-growth conditions using a horizontal Bridgman furnace and square glass ampoule. For use as input boundary conditions to numerical codes, thermal profiles on the outside of the ampoule at five locations around its periphery were measured along the ampoule's length. Temperatures inside the ampoule were also measured. The shapes of the s/l interface in various two dimensional planes were quantitatively determined. Though interfaces were nondendritic and noncellular, they were not flat, but were highly curved and symmetric in only one unique longitudinal y-z plane (at x=O). The shapes of the interface were dominated by the primary longitudinal flow cell characteristic of shallow cavity flow in horizontal Bridgman; this flow cell was driven by the imposed furnace temperature gradient and caused a 'radical' thermal gradient such that the upper half of the ampoule was hotter than the bottom half. We believe that due to the strong convection, the release of latent heat does not significantly influence the thermal conditions near the interface. We hope that the interface shape and thermal data presented in this paper can be used to optimize crystal growth processes and validate numerical models.

Methods of viscosity measurements in sealed ampoules

NASA Astrophysics Data System (ADS)

Mazuruk, Konstantin

1999-07-01

Viscosity of semiconductors and metallic melts is usually measured by oscillating cup method. This method utilizes the melts contained in vacuum sealed silica ampoules, thus the problems related to volatility, contamination, and high temperature and pressure can be alleviate. In a typical design, the time required for a single measurement is of the order of one hour. In order to reduce this time to a minute range, a high resolution angular detection system is implemented in our design of the viscometer. Furthermore, an electromagnet generating a rotational magnetic field (RMF) is incorporated into the apparatus. This magnetic field can be used to remotely and nonintrusively measure the electrical conductivity of the melt. It can also be used to induce a well controlled rotational flow in the system. The transient behavior of this flow can potentially yield of the fluid. Based on RMF implementation, two novel viscometry methods are proposed in this work: a) the transient torque method, b) the resonance method. A unified theoretical approach to the three methods is presented along with the initial test result of the constructed apparatus. Advantages of each of the method are discussed.

Glass sealing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brow, R.K.; Kovacic, L.; Chambers, R.S.

1996-04-01

Hernetic glass sealing technologies developed for weapons component applications can be utilized for the design and manufacture of fuel cells. Design and processing of of a seal are optimized through an integrated approach based on glass composition research, finite element analysis, and sealing process definition. Glass sealing procedures are selected to accommodate the limits imposed by glass composition and predicted calculations.

Titanium sealing glasses and seals formed therefrom

DOEpatents

Brow, Richard K.; McCollister, Howard L.; Phifer, Carol C.; Day, Delbert E.

1997-01-01

Alkaline-earth lanthanoborate sealing-glass compositions containing CaO, La.sub.2 O.sub.3, B.sub.2 O.sub.3, TiO.sub.2 and Al.sub.2 O.sub.3 in various combinations of mole-% are provided. These sealing-glass compositions are useful for forming hermetic glass-to-metal seals with titanium and titanium alloys that have a high aqueous durability for component or device applications requiring exposure to moisture, water or body fluids. Particular applications of the titanium sealing-glass compositions include forming glass-to-metal seals for lithium batteries and implanted biomedical devices (e.g. batteries, pacemakers, defibrillators, pumps).

Pre-filled syringe - a ready-to-use drug delivery system: a review.

PubMed

Ingle, Rahul G; Agarwal, Aayush S

2014-09-01

Fueled by a growing global expectation of the health and medical fields, billions of dollars/euros/pounds are invested every year in the research of new biological and chemical entities. However, little interest is seen in the development of novel drug delivery systems. One such system, pre-filled syringe (PFS), was invented decades ago but is still a rare mode of delivery in many therapeutic segments. This review comprises properties and effects of extractables, leachables and discuss the characteristics of PFS technology; its composition, glass and polymer types, configuration of PFS, advantages over glass, technical and commercial applicability; its significance against patient, industry, quality, environment and cost; and its business potential. We discuss in brief about PFS used in various major and life-threatening disorders and future prospects. It provides showers of knowledge in the field of PFS drug delivery technology to the reader's, industrialist's and researcher's point of view. The PFS drug delivery system offers a wonderful panorama to lifesaving drugs that are currently only available in conventional vials and ampoules in the market. A novel approach of Form Fill Seal technology can be adopted for this particular ready-to-use dosage form also, which opens the new global doors for budding researchers in the field of pre-filled drug delivery system.

Titanium sealing glasses and seals formed therefrom

DOEpatents

Brow, R.K.; McCollister, H.L.; Phifer, C.C.; Day, D.E.

1997-12-02

Alkaline-earth lanthanoborate sealing-glass compositions containing CaO, La{sub 2}O{sub 3}, B{sub 2}O{sub 3}, TiO{sub 2} and Al{sub 2}O{sub 3} in various combinations of mole-% are provided. These sealing-glass compositions are useful for forming hermetic glass-to-metal seals with titanium and titanium alloys that have a high aqueous durability for component or device applications requiring exposure to moisture, water or body fluids. Particular applications of the titanium sealing-glass compositions include forming glass-to-metal seals for lithium batteries and implanted biomedical devices (e.g. batteries, pacemakers, defibrillators, pumps). 2 figs.

Interface Lattice Engineering of Si Composite Wafers for Large-Format HgCdTe Infrared Focal Plane Arrays

DTIC Science & Technology

2012-08-07

sealed quartz ampoule under a mercury overpressure in a conventional clam-shell furnace . The reduction in the dislocation density has been studied as...46 2.6.4 Etch Pit Characterization . . . . . . . . . . . . . . . . . . . . . . . . 46 5 3 Furnace Setup and Calibration...Setup . . . . . . . . . . . . . . . . . . . . . . . 54 3.1.2 Furnace Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . 55 4 In Situ

Validation Assessment of a Glass-to-Metal Seal Finite-Element Model

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jamison, Ryan Dale; Buchheit, Thomas E.; Emery, John M

Sealing glasses are ubiquitous in high pressure and temperature engineering applications, such as hermetic feed-through electrical connectors. A common connector technology are glass-to-metal seals where a metal shell compresses a sealing glass to create a hermetic seal. Though finite-element analysis has been used to understand and design glass-to-metal seals for many years, there has been little validation of these models. An indentation technique was employed to measure the residual stress on the surface of a simple glass-to-metal seal. Recently developed rate- dependent material models of both Schott 8061 and 304L VAR stainless steel have been applied to a finite-element modelmore » of the simple glass-to-metal seal. Model predictions of residual stress based on the evolution of material models are shown. These model predictions are compared to measured data. Validity of the finite- element predictions is discussed. It will be shown that the finite-element model of the glass-to-metal seal accurately predicts the mean residual stress in the glass near the glass-to-metal interface and is valid for this quantity of interest.« less

Method of forming shrink-fit compression seal

NASA Technical Reports Server (NTRS)

Podgorski, T. J. (Inventor)

1977-01-01

A method for making a glass-to-metal seal is described. A domed metal enclosure having a machined seal ring is fitted to a glass post machined to a slight taper and to a desired surface finish. The metal part is then heated by induction in a vacuum. As the metal part heats and expands relative to the glass post, the metal seal ring, possessing a higher coefficient of expansion than the glass post, slides down the tapered post. Upon cooling, the seal ring crushes against the glass post forming the seal. The method results in a glass-to-metal seal possessing extremely good leak resistance, while the parts are kept clean and free of the contaminants.

The Isonzo front in the First World War: glass ampoules found in the vicinity of the village Kred.

PubMed

Krbavcic, Ales

2015-01-01

To identify the contents of ampoules stored items at the WW I Kobarid Museum, Slovenia. Sources and methods: Analysis of ampoules from the Kobarid Museum using pharmacopoeial methods. The contents of the unlabelled ampoules were identified as calcium hypochlorite, a decontaminant for mustard gas (Yperite). The Isonzo front/Soška fronta was opened on May 24 1915 by the Kingdom of Italy according to a secret London Treaty. In exchange for the opening of this front, the Kingdom of Italy would be granted large tracts of territory in the wesster provinces of the Austro-Hungarian Empire and along the Adriatic coast. The ensuing trench-warfare during the eleven Isonzo battles ended with the 12th battle known as the Kobarid/Karfeit/Caporetto break-thru in October 1917. The joint German and Austro-Hungarian forces waged a massive gas-attack with dichloroarsine and phosgene, which was later disclosed as the horrifying overture to the general disordered retreat of the Italian troops to Piave. The possibility of a chemical attack was underestimated by the Italian high command as shown by the ineffective gas-masks issued to the troops. Hovewer, a recent find of ampoules with calcium hypochlorite at the village of Kred, now exhibited at the Kobarid WWI Museum, leads to the conclusion that the Italian IVth army's command, located in Kred, considered decontamination measures against Yperite necessary.

Theory and Simulation of A Novel Viscosity Measurement Method for High Temperature Semiconductor

NASA Technical Reports Server (NTRS)

Lin, Bochuan; Li, Chao; Ban, Heng; Scripa, Rose; Zhu, Shen; Su, Ching-Hua; Lehoczky, S. L.; Curreri, Peter A. (Technical Monitor)

2002-01-01

The properties of molten semiconductors are good indicators for material structure transformation and hysteresis under temperature variations. Viscosity, as one of the most important properties, is difficult to measure because of high temperature, high pressure, and vapor toxicity of melts. Recently, a novel method was developed by applying a rotating magnetic field to the melt sealed in a suspended quartz ampoule, and measuring the transient torque exerted by rotating melt flow on the ampoule wall. The method was designed to measure viscosity in short time period, which is essential for evaluating temperature hysteresis. This paper compares the theoretical prediction of melt flow and ampoule oscillation with the experimental data. A theoretical model was established and the coupled fluid flow and ampoule torsional vibration equations were solved numerically. The simulation results showed a good agreement with experimental data. The results also showed that both electrical conductivity and viscosity could be calculated by fitting the theoretical results to the experimental data. The transient velocity of the melt caused by the rotating magnetic field was found reach equilibrium in about half a minute, and the viscosity of melt could be calculated from the altitude of oscillation. This would allow the measurement of viscosity in a minute or so, in contrast to the existing oscillation cup method, which requires about an hour for one measurement.

Science Officer Whitson installs SUBSA in MSG

NASA Image and Video Library

2002-07-05

ISS005-E-06787 (5 July 2002) --- Astronaut Peggy A. Whitson, Expedition Five flight engineer, works near the Microgravity Science Glovebox (MSG) in the Destiny laboratory on the International Space Station (ISS). Whitson spent much of the morning installing the Solidification Using a Baffle in Sealed Ampoules (SUBSA) experiment in the MSG. The SUBSA installation will be completed once the MSG is activated.

Methods of Viscosity Measurements in Sealed Ampoules

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin

1999-01-01

Viscosity of semiconductor and metallic melts is usually measured by oscillating cup method. This method utilizes the melts contained in vacuum sealed silica ampoules, thus the problems related to volatility, contamination, and high temperature and pressure can be alleviated. In a typical design, the time required for a single measurement is of the order of one hour. In order to reduce this time to a minute range, a high resolution (0.05 arc.sec) angular detection system is implemented in our design of the viscometer. Furthermore, an electromagnet generating a rotational magnetic field (RMF) is incorporated into the apparatus. This magnetic field can be used to remotely and non intrusively measure the electrical conductivity of the melt. It can also be used to induce a well controlled rotational flow in the system. The transient behavior of this flow can potentially yield the viscosity of the fluid. Based on RMF implementation, two novel viscometry methods are proposed in this work: a) the transient torque method, b) the resonance method. A unified theoretical approach to the three methods (oscillating cup, transient torque, and resonance) is presented along with the initial test results of the constructed apparatus. Advantages of each of the method are discussed.

Production of glass or glass-ceramic to metal seals with the application of pressure

DOEpatents

Kelly, Michael D.; Kramer, Daniel P.

1987-11-10

In a process for preparing a glass or glass-ceramic to metal seal comprising contacting the glass with the metal and heat-treating the glass and metal under conditions whereby the glass to metal seal is effected and, optionally, the glass is converted to a glass-ceramic, an improvement comprises carrying out the heat-treating step using hot isostatic pressing.

Production of glass or glass-ceramic to metal seals with the application of pressure

DOEpatents

Kelly, M.D.; Kramer, D.P.

1985-01-04

In a process for preparing a glass or glass-ceramic to metal seal comprising contacting the glass with the metal and heat-treating the glass and metal under conditions whereby the glass to metal seal is effected and, optionally, the glass is converted to a glass-ceramic, an improvement comprises carrying out the heat-treating step using hot isostatic pressing.

Alternate seal configuration for lithium primary cells

NASA Technical Reports Server (NTRS)

Kelley, J. A.

1982-01-01

The problem of glass degradation in the glass-to-metal seals in lithium/sulfur dioxide cells is discussed. The glass degradation mechanism is attributed to lithium reacting with glass which is a result of deposition of lithium at the glass/metal/electrolyte interface. The worst degradation was observed when cells were stored in the inverted position. Alternate sealing methods were examined and a modified Ziegler seal is considered to be one of the best possible methods. The seal consists of a crimp type soft seal using a plastic annulus and a metal tube. Results of degradation tests are presented.

24 CFR 200.940 - Supplementary specific requirements under the HUD building product standards and certification...

Code of Federal Regulations, 2011 CFR

2011-04-01

... under the HUD building product standards and certification program for sealed insulating glass units... sealed insulating glass units. (a) Applicable standards. (1) All sealed insulating glass units shall be... standard: ASTM E-774-92 Standard Specification for Sealed Insulating Glass Units. (2) This standard has...

24 CFR 200.940 - Supplementary specific requirements under the HUD building product standards and certification...

Code of Federal Regulations, 2010 CFR

2010-04-01

... under the HUD building product standards and certification program for sealed insulating glass units... sealed insulating glass units. (a) Applicable standards. (1) All sealed insulating glass units shall be... standard: ASTM E-774-92 Standard Specification for Sealed Insulating Glass Units. (2) This standard has...

Method for producing ceramic-glass-ceramic seals by microwave heating

DOEpatents

Blake, Rodger D.; Meek, Thomas T.

1986-01-01

Method for producing a ceramic-glass-ceramic seal by the use of microwave energy, and a sealing mixture which comprises a glass sealing material, a coupling agent, and an oxidizer. The seal produced exhibits greater strength due to its different microstructure. Sodium nitrate is the most preferred oxidizer.

Stress Mapping in Glass-to-Metal Seals using Indentation Crack Lengths.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Strong, Kevin; Buchheit, Thomas E.; Diebold, Thomas Wayne

Predicting the residual stress which develops during fabrication of a glass-to-metal compression seal requires material models that can accurately predict the effects of processing on the sealing glass. Validation of the predictions requires measurements on representative test geometries to accurately capture the interaction between the seal materials during a processing cycle required to form the seal, which consists of a temperature excursion through the glass transition temperature of the sealing glass. To this end, a concentric seal test geometry, referred to as a short cylinder seal, consisting of a stainless steel shell enveloping a commercial sealing glass disk has beenmore » designed, fabricated, and characterized as a model validation test geometry. To obtain data to test/validate finite element (FE) stress model predictions of this geometry, spatially-resolved residual stress was calculated from the measured lengths of the cracks emanating from radially positioned Vickers indents in the glass disk portion of the seal. The indentation crack length method is described, and the spatially-resolved residual stress determined experimentally are compared to FE stress predictions made using a nonlinear viscoelastic material model adapted to inorganic sealing glasses and an updated rate dependent material model for 304L stainless steel. The measurement method is a first to achieve a degree of success for measuring spatially resolved residual stress in a glass-bearing geometry and a favorable comparison between measurements and simulation was observed.« less

Stress Mapping in Glass-to-Metal Seals using Indentation Crack Lengths

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buchheit, Thomas E.; Strong, Kevin; Newton, Clay S.

Predicting the residual stress which develops during fabrication of a glass-to-metal compression seal requires material models that can accurately predict the effects of processing on the sealing glass. Validation of the predictions requires measurements on representative test geometries to accurately capture the interaction between the seal materials during a processing cycle required to form the seal, which consists of a temperature excursion through the glass transition temperature of the sealing glass. To this end, a concentric seal test geometry, referred to as a short cylinder seal, consisting of a stainless steel shell enveloping a commercial sealing glass disk has beenmore » designed, fabricated, and characterized as a model validation test geometry. To obtain data to test/validate finite element (FE) stress model predictions of this geometry, spatially-resolved residual stress was calculated from the measured lengths of the cracks emanating from radially positioned Vickers indents in the glass disk portion of the seal. The indentation crack length method is described, and the spatially-resolved residual stress determined experimentally are compared to FE stress predictions made using a nonlinear viscoelastic material model adapted to inorganic sealing glasses and an updated rate dependent material model for 304L stainless steel. The measurement method is a first to achieve a degree of success for measuring spatially resolved residual stress in a glass-bearing geometry and a favorable comparison between measurements and simulation was observed.« less

Simultaneous in situ Optical Monitoring Techniques during Crystal Growth of ZnSe by Physical Vapor Transport

NASA Technical Reports Server (NTRS)

Su, C.- H.; Feth, S.; Lehoczky, S. L.

1998-01-01

ZnSe crystals grown in sealed ampoules by the physical vapor transport method were monitored in situ using three techniques, simultaneously. A Michelson interferometer was set-up to observe the growth rate and surface morphological evolution. An interference pattern (interferogram) is formed by the interaction between the reflection of a HeNe laser (632.8 nm wavelength) off the crystal-vapor interface and a reference beam from the same laser. Preliminary results indicate that the rate of growth/thermal-etching can be calculated using analog data acquisition and simple fringe counting techniques. Gross surface features may also be observed using a digital frame grabber and fringe analysis software. The second in situ technique uses optical absorption to determine the partial pressures of the vapor species. The Se2 and Zn vapor species present in the sealed ampoule absorb light at characteristic wavelengths. The optical absorption is determined by monitoring the light intensity difference between the sample and reference beams. The Se2 Partial pressure profile along the length of the ampoule was estimated from the vibronic absorption peaks at 340.5, 350.8, 361.3 and 379.2 nm using the Beer's law constants established in the calibration runs of pure Se. Finally, because the high temperature crystal growth furnace contains windows, in situ visual observation of the growing crystal is also possible. The use of these techniques not only permits in situ investigation of high temperature vapor growth of semiconductors, but also offers the potential for real time feed back on the growing crystal and allows the possibility of actively controlling the growth process.

A mononuclear iron(II) complex: cooperativity, kinetics and activation energy of the solvent-dependent spin transition.

PubMed

Bushuev, Mark B; Pishchur, Denis P; Logvinenko, Vladimir A; Gatilov, Yuri V; Korolkov, Ilya V; Shundrina, Inna K; Nikolaenkova, Elena B; Krivopalov, Viktor P

2016-01-07

The system [FeL2](BF4)2 (1)-EtOH-H2O (L is 4-(3,5-dimethyl-1H-pyrazol-1-yl)-2-(pyridin-2-yl)-6-methylpyrimidine) shows a complicated balance between the relative stabilities of solvatomorphs and polymorphs of the complex [FeL2](BF4)2. New solvatomorphs, 1(LS)·EtOH·H2O and β-1(LS)·xH2O, were isolated in this system. They were converted into four daughter phases, 1(A/LS), 1(D/LS), 1(E/LS)·yEtOH·zH2O and 1(F/LS). On thermal cycling in sealed ampoules, the phases 1(LS)·EtOH·H2O and β-1(LS)·xH2O transform into the anhydrous phase 1(A/LS). The hysteresis loop width for the (A/LS) ↔ (A/HS) spin transition depends on the water and ethanol contents in the ampoule and varies from ca. 30 K up to 145 K. The reproducible hysteresis loop of 145 K is the widest ever reported one for a spin crossover complex. The phase 1(A/LS) combines the outstanding spin crossover properties with thermal robustness allowing for multiple cycling in sealed ampoules without degradation. The kinetics of the 1(A/LS) → 1(A/HS) transition is sigmoidal which is indicative of strong cooperative interactions. The cooperativity of the 1(A/LS) → 1(A/HS) transition is related to the formation of a 2D supramolecular structure of the phase 1(A/LS). The activation energy for the spin transition is very high (hundreds of kJ mol(-1)). The kinetics of the 1(A/HS) → 1(A/LS) transition can either be sigmoidal or exponential depending on the water and ethanol contents in the ampoule. The phases 1(D/LS) and 1(F/LS) show gradual crossover, whereas the phase 1(E/LS)·yEtOH·yH2O shows a reversible hysteretic transition associated with the solvent molecule release and uptake.

Heterogeneous nucleation of aspartame from aqueous solutions

NASA Astrophysics Data System (ADS)

Kubota, Noriaki; Kinno, Hiroaki; Shimizu, Kenji

1990-03-01

Waiting times, the time from the instant of quenching needed for a first nucleus to appear, were measured at constant supercoolings for primary nucleation of aspartame (α-L-aspartyl-L-phenylalanine methylester) from aqueous solutions, which were sealed into glass ampoules (solution volume = 3.16 cm 3). Since the waiting time became shorter by filtering the solution prior to quenching, the nucleation was concluded to be heterogeneously induced. The measured waiting time consisted of two parts: time needed for the nucleus to grow to a detactable size (growth time) and stochastic time needed for nucleation (true waiting time). The distribution of the true waiting time, is well explained by a stochastic model, in which nucleation is regarded to occur heterogeneously and in a stochastic manner by two kinds of active sites. The active sites are estimated to be located on foreign particles in which such elements as Si, Al and Mg were contained. The amount of each element is very small in the order of magnitude of ppb (mass basis) of the whole solution. The growth time was correlated with the degree of supercooling.

Solder glass sealing technology for use in packaging of fiber optic sensors

NASA Astrophysics Data System (ADS)

Kreutzmann, Gerd

1990-08-01

The solder glass sealing technology is an alternative to the direct sealing method of the socalled hboptocansu. Using solder glass for the junction of glass and the metal can the temperature at about 500 °C does not destroy the optical quality of the precision glass components. The glass can also be coated with an antireflective layer and even the sealing of filterglass is possible. In cases where coupling losses can't be tolerated, the fiber has to be fed directly through the wall into the housing. Fiber feedthroughs, using solder glass for the sealing of the fiber into a metal tube, are commonly metal soldered or welded into the wall and the fiber surface is directly leading to the semiconductor.

Laser sealed vacuum insulation window

DOEpatents

Benson, David K.; Tracy, C. Edwin

1987-01-01

A laser sealed evacuated window panel is comprised of two glass panes held spaced apart in relation to each other by a plurality of spherical glass beads and glass welded around the edges to provide an evacuated space between the glass panes that is completely glass sealed from the exterior. The glass welded edge seal is obtained by welding the edges of the glass panes together with a laser beam while the glass panes and bead spacers are positioned in a vacuum furnace and heated to the annealing point of the glass to avoid stress fracture in the area of the glass weld. The laser welding in the furnace can be directed around the perimeter of the glass panel by a combination of rotating the glass panel and linearly translating or aiming the laser with a relay mirror.

Ceramic-glass-metal seal by microwave heating

DOEpatents

Meek, Thomas T.; Blake, Rodger D.

1985-01-01

A method for producing a ceramic-glass-metal seal by microwaving mixes a slurry of glass sealing material and coupling agent and applies same to ceramic and metal workpieces. The slurry and workpieces are then insulated and microwaved at a power, time and frequency sufficient to cause a liquid phase reaction in the slurry. The reaction of the glass sealing material forms a chemically different seal than that which would be formed by conventional heating because it is formed by diffusion rather than by wetting of the reactants.

Ceramic-glass-metal seal by microwave heating

DOEpatents

Meek, T.T.; Blake, R.D.

1983-10-04

A method for producing a ceramic-glass-metal seal by microwaving, mixes a slurry of glass sealing material and coupling agent and applies same to ceramic and metal workpieces. The slurry and workpieces are then insulated and microwaved at a power, time and frequency sufficient to cause a liquid-phase reaction in the slurry. The reaction of the glass sealing material forms a chemically different seal than that which would be formed by conventional heating because it is formed by diffusion rather than by wetting of the reactants.

The growth of zinc selenide single crystals by physical vapor transport in microgravity

NASA Technical Reports Server (NTRS)

Anderson, Elmer E.; Rosenberger, Franz E.; Cheng, Hai-Yuin

1990-01-01

Growth and characterization studies will be performed on zinc selenide single crystals. The high temperature outgassing behavior of the silica ampoule material will be studied in order to develop a cleaning and bake-out procedure that will minimize the amount of impurities introduced into the vapor from the ampoule materials and in particular during the seal-off procedure. The outgassing behavior of the ZnSe starting material will be studied during high vacuum refinement at elevated temperatures in order to develop a temperature pressure program that will optimize the removal of impurities while minimizing a shift in stoichiometry due to preferred evaporation of the higher fugacity component. The mass spectrometer system was completed, and after calibration, will be used to perform the above tasks. The system and its operation is described in detail.

Glass formation and short-range order structures in the BaS + La 2S 3 + GeS 2 system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roth, Josh R.; Martin, Steve W.; Ballato, John

Here, infrared (IR) optical materials have enabled a broad range of optical sensing and measurement applications in the mid-wave and long-wave IR. Many IR transmitting glasses are based on covalently-bonded selenides and tellurides, such as As 2Se 3 and GeTe 2, which typically have relatively low glass transition temperatures ( T g) on the order of 200 to 350 °C. Many applications have working temperatures above the T g of these materials, which compels the development of new IR materials. This work studies the underlying short-range order (SRO) structure and glass formability of a new family of ionically-bonded sulfide glasses,more » xBaS + yLa 2S 3 + (1 – x – y)GeS 2, to develop high T g optical materials with a broad IR transmission range. These sulfide glasses were produced by melting sulfide materials inside evacuated and sealed carbon-coated silica ampoules at 1150 °C for 12 h and quenching to room temperature to form glass. Glass samples were then characterized by IR and Raman spectroscopies and differential thermal analysis (DTA). It was found that by increasing the modifier concentration, the predominantly Ge 4 SRO units, the superscript defines the number of bridging sulfur (BS) ions in the tetrahedral network found in GeS 2 glasses, are ultimately converted to Ge 0 units at >40 mol% network modifier content through the generation of non-bridging sulfur (NBS) ions. These molecular ionic units still form a glassy network, with some of the highest reported T g values to date for a pure sulfide glass. This suggests that this composition has strong ionic bonds between negatively-charged tetrahedral SRO units and the positively-charged modifier cations. While the glass network is depolymerized in the high modifier content glasses though the formation of a high concentration of molecular ionic Ge 0 SRO groups, they are, nevertheless, homogeneous glassy materials that exhibit the largest T g and Δ T (difference between crystallization temperature, T c, and T g) values of glasses in this system, making them the optimal glasses for high T g IR optical components, including, potentially, refractory IR optical fibers.« less

Glass formation and short-range order structures in the BaS + La 2S 3 + GeS 2 system

DOE PAGES

Roth, Josh R.; Martin, Steve W.; Ballato, John; ...

2018-06-01

Here, infrared (IR) optical materials have enabled a broad range of optical sensing and measurement applications in the mid-wave and long-wave IR. Many IR transmitting glasses are based on covalently-bonded selenides and tellurides, such as As 2Se 3 and GeTe 2, which typically have relatively low glass transition temperatures ( T g) on the order of 200 to 350 °C. Many applications have working temperatures above the T g of these materials, which compels the development of new IR materials. This work studies the underlying short-range order (SRO) structure and glass formability of a new family of ionically-bonded sulfide glasses,more » xBaS + yLa 2S 3 + (1 – x – y)GeS 2, to develop high T g optical materials with a broad IR transmission range. These sulfide glasses were produced by melting sulfide materials inside evacuated and sealed carbon-coated silica ampoules at 1150 °C for 12 h and quenching to room temperature to form glass. Glass samples were then characterized by IR and Raman spectroscopies and differential thermal analysis (DTA). It was found that by increasing the modifier concentration, the predominantly Ge 4 SRO units, the superscript defines the number of bridging sulfur (BS) ions in the tetrahedral network found in GeS 2 glasses, are ultimately converted to Ge 0 units at >40 mol% network modifier content through the generation of non-bridging sulfur (NBS) ions. These molecular ionic units still form a glassy network, with some of the highest reported T g values to date for a pure sulfide glass. This suggests that this composition has strong ionic bonds between negatively-charged tetrahedral SRO units and the positively-charged modifier cations. While the glass network is depolymerized in the high modifier content glasses though the formation of a high concentration of molecular ionic Ge 0 SRO groups, they are, nevertheless, homogeneous glassy materials that exhibit the largest T g and Δ T (difference between crystallization temperature, T c, and T g) values of glasses in this system, making them the optimal glasses for high T g IR optical components, including, potentially, refractory IR optical fibers.« less

Laser Glass Frit Sealing for Encapsulation of Vacuum Insulation Glasses

NASA Astrophysics Data System (ADS)

Kind, H.; Gehlen, E.; Aden, M.; Olowinsky, A.; Gillner, A.

Laser glass frit sealing is a joining method predestined in electronics for the sealing of engineered materials housings in dimensions of some 1 mm2 to several 10 mm2. The application field ranges from encapsulation of display panels to sensor housings. Laser glass frit sealing enables a hermetical closure excluding humidity and gas penetration. But the seam quality is also interesting for other applications requiring a hermetical sealing. One application is the encapsulation of vacuum insulation glass. The gap between two panes must be evacuated for reducing the thermal conductivity. Only an efficient encapsulating technique ensures durable tight joints of two panes for years. Laser glass frit sealing is an alternative joining method even though the material properties of soda lime glass like sensitivity to thermal stresses are much higher as known from engineered materials. An adapted thermal management of the process is necessary to prevent the thermal stresses within the pane to achieve crack free and tight glass frit seams.

Transient Torque Method: A Fast and Non-Intrusive Technique to Simultaneously Determine Viscosity and Electrical Conductivity of Semiconducting and Metallic Melts

NASA Technical Reports Server (NTRS)

Li, C.; Ban, H.; Lin, B.; Scripa, R. N.; Su, C.; Lehoczky, S. L.; Zhu, S.

2003-01-01

A transient torque method was developed to rapidly and simultaneously determine the viscosity and electrical conductivity of semiconducting or metallic melts. The experimental setup is similar to that for the oscillation cup technique. The melt sample is sealed inside a fused silica ampoule, and the ampoule is suspended by a long quartz fiber to form a torsional oscillation system. A rotating magnetic field is used to induce a rotating flow in the conductive melt, which causes the ampoule to rotate along its axis. A sensitive angular detector is used to measure the deflection angle of the ampoule. Based on the transient behavior of the deflection angle as the rotating magnetic field is applied, the electrical conductivity and viscosity of the melt can be obtained simultaneously by numerically fitting the data to a set of governing equations. The transient torque viscometer was applied successfully to measure the viscosity and electrical conductivity of high purity mercury at 53.4 C. The results were in excellent agreement with the published data. The main advantage of the technique is that the measurement can be completed in one or two minutes, as opposed to the one or two-hour measurement time required by the oscillation cup technique. The method is non-intrusive; capable of rapid measurement of the viscosity of toxic, high vapor pressure melts at elevated temperatures. In addition, the transient torque viscometer can also be operated as an oscillation cup viscometer if desired.

Transient Torque Method: A Fast and Nonintrusive Technique to Simultaneously Determine Viscosity and Electrical Conductivity of Semiconducting and Metallic Melts

NASA Technical Reports Server (NTRS)

Li, C.; Ban, H.; Lin, B.; Scripa, R. N.; Su, C.-H.; Lehoczky, S. L.; Zhu, S.

2004-01-01

A transient torque method was developed to rapidly and simultaneously determine the viscosity and electrical conductivity of liquid metals and molten semiconductors. The experimental setup of the transient torque method is similar to that of the oscillation cup method. The melt sample is sealed inside a fused silica ampoule, and the ampoule is suspended by a long quartz fiber to form a torsional oscillation system. A rotating magnetic field is used to induce a rotating flow in the conductive melt, which causes the ampoule to rotate around its vertical axis. A sensitive angular detector is used to measure the deflection angle of the ampoule. Based on the transient behavior of the deflection angle as the rotating magnetic field is applied, the electrical conductivity and viscosity of the melt can be obtained simultaneously by numerically fitting the data to a set of governing equations. The transient torque viscometer was applied successfully to measure the viscosity and electrical conductivity of high purity mercury at 53.4 C. The results were in excellent agreement with published data. The method is nonintrusive; capable of rapid measurement of the viscosity of toxic, high vapor pressure melts at elevated temperatures. In addition, the transient torque viscometer can also be operated as an oscillation cup viscometer to measure just the viscosity of the melt or as a rotating magnetic field method to determine the electrical conductivity of a melt or a solid if desired.

Laser sealed vacuum insulating window

DOEpatents

Benson, D.K.; Tracy, C.E.

1985-08-19

A laser sealed evacuated window panel is comprised of two glass panes held spaced apart in relation to each other by a plurality of spherical glass beads and glass welded around the edges to provide an evacuated space between the glass panes that is completely glass sealed from the exterior. The glass welded edge seal is obtained by welding the edges of the glass panes together with a laser beam while the glass panes and bead spacers are positioned in a vacuum furnace and heated to the annealing point of the glass to avoid stress fracture in the area of the glass weld. The laser welding in the furnace can be directed around the perimeter of the galss panel by a combination of rotating the glass panel and linearly translating or aiming the laser with a relay mirror.

Ceramic-glass-ceramic seal by microwave heating

DOEpatents

Meek, T.T.; Blake, R.D.

1983-10-04

A method for producing a ceramic-glass-ceramic seal by microwaving, mixes a slurry of glass sealing material and coupling agent and applies same to ceramic workpieces. The slurry and workpieces are placed together, insulated and then microwaved at a power, time and frequency sufficient to cause a liquid phase reaction in the slurry. The reaction of the glass sealing material forms a chemically different seal than that which would be formed by conventional heating because it is formed by a diffusion rather than by wetting of the reactants.

Ceramic-glass-ceramic seal by microwave heating

DOEpatents

Meek, Thomas T.; Blake, Rodger D.

1985-01-01

A method for producing a ceramic-glass-ceramic seal by microwaving, mixes a slurry of glass sealing material and coupling agent and applies same to ceramic workpieces. The slurry and workpieces are placed together, insulated and then microwaved at a power, time and frequency sufficient to cause a liquid phase reaction in the slurry. The reaction of the glass sealing material forms a chemically different seal than that which would be formed by conventional heating because it is formed by a diffusion rather than by wetting of the reactants.

Sealing glasses for titanium and titanium alloys

DOEpatents

Brow, R.K.; McCollister, H.L.; Phifer, C.C.; Day, D.E.

1997-07-15

Barium lanthanoborate sealing-glass compositions are provided comprising various combinations (in terms of mole-%) of boron oxide (B{sub 2}O{sub 3}), barium oxide (BaO), lanthanum oxide (La{sub 2}O{sub 3}), and at least one other oxide selected from the group consisting of aluminum oxide (Al{sub 2}O{sub 3}), calcium oxide (CaO), lithium oxide (Li{sub 2}O), sodium oxide (Na{sub 2}O), silicon dioxide (SiO{sub 2}), or titanium dioxide (TiO{sub 2}). These sealing-glass compositions are useful for forming hermetic glass-to-metal seals with titanium and titanium alloys having an improved aqueous durability and favorable sealing characteristics. Examples of the sealing-glass compositions are provided having coefficients of thermal expansion about that of titanium or titanium alloys, and with sealing temperatures less than about 900 C, and generally about 700--800 C. The barium lanthanoborate sealing-glass compositions are useful for components and devices requiring prolonged exposure to moisture or water, and for implanted biomedical devices (e.g. batteries, pacemakers, defibrillators, pumps). 1 fig.

Sealing glasses for titanium and titanium alloys

DOEpatents

Brow, Richard K.; McCollister, Howard L.; Phifer, Carol C.; Day, Delbert E.

1997-01-01

Barium lanthanoborate sealing-glass compositions are provided comprising various combinations (in terms of mole-%) of boron oxide (B.sub.2 O.sub.3), barium oxide (BaO), lanthanum oxide (La.sub.2 O.sub.3), and at least one other oxide selected from the group consisting of aluminum oxide (Al.sub.2 O.sub.3), calcium oxide (CaO), lithium oxide (Li.sub.2 O), sodium oxide (Na.sub.2 O), silicon dioxide (SiO.sub.2), or titanium dioxide (TiO.sub.2). These sealing-glass compositions are useful for forming hermetic glass-to-metal seals with titanium and titanium alloys having an improved aqueous durability and favorable sealing characteristics. Examples of the sealing-glass compositions are provided having coefficients of thermal expansion about that of titanium or titanium alloys, and with sealing temperatures less than about 900.degree. C., and generally about 700.degree.-800.degree. C. The barium lanthanoborate sealing-glass compositions are useful for components and devices requiring prolonged exposure to moisture or water, and for implanted biomedical devices (e.g. batteries, pacemakers, defibrillators, pumps).

Sealing glasses for titanium and titanium alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brow, R.K.; McCollister, H.L.; Phifer, C.C.

1997-07-15

Barium lanthanoborate sealing-glass compositions are provided comprising various combinations (in terms of mole-%) of boron oxide (B{sub 2}O{sub 3}), barium oxide (BaO), lanthanum oxide (La{sub 2}O{sub 3}), and at least one other oxide selected from the group consisting of aluminum oxide (Al{sub 2}O{sub 3}), calcium oxide (CaO), lithium oxide (Li{sub 2}O), sodium oxide (Na{sub 2}O), silicon dioxide (SiO{sub 2}), or titanium dioxide (TiO{sub 2}). These sealing-glass compositions are useful for forming hermetic glass-to-metal seals with titanium and titanium alloys having an improved aqueous durability and favorable sealing characteristics. Examples of the sealing-glass compositions are provided having coefficients of thermal expansionmore » about that of titanium or titanium alloys, and with sealing temperatures less than about 900 C, and generally about 700--800 C. The barium lanthanoborate sealing-glass compositions are useful for components and devices requiring prolonged exposure to moisture or water, and for implanted biomedical devices (e.g. batteries, pacemakers, defibrillators, pumps). 1 fig.« less

Study of Geometric Stability and Structural Integrity of Self-Healing Glass Seal System Used in Solid Oxide Fuel Cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Wenning N.; Sun, Xin; Khaleel, Mohammad A.

A self-healing glass seal has the potential of restoring its mechanical properties upon being reheated to SOFC stack operating temperature, even when it has experienced some cooling induced damage/cracking at room temperature. Such a self-healing feature is desirable for achieving high seal reliability during thermal cycling. On the other hand, self-healing glass is also characterized by its low mechanical stiffness and high creep rate at the typical operating temperature of SOFCs. Therefore, geometry stability and structural integrity of the glass seal system becomes critical to its successful application in SOFCs. In this paper, the geometry stability of the self-healing glassmore » and the influence of various interfacial conditions of ceramic stoppers with the PEN, IC, and glass seal on the structural integrity of the glass seal during the operating and cooling down processes are studied using finite element analyses. For this purpose, the test cell used in the leakage tests for compliant glass seals conducted at PNNL is taken as the initial modeling geometry. The effect of the ceramic stopper on the geometry stability of the self-healing glass sealants is studied first. Two interfacial conditions of the ceramic stopper and glass seals, i.e., bonded (strong) or un-bonded (weak), are considered. Then the influences of interfacial strengths at various interfaces, i.e., stopper/glass, stopper/PEN, as well as stopper/IC plate, on the geometry stability and reliability of glass during the operating and cooling processes are examined.« less

Ionic requirements for membrane-glass adhesion and giga seal formation in patch-clamp recording.

PubMed

Priel, Avi; Gil, Ziv; Moy, Vincent T; Magleby, Karl L; Silberberg, Shai D

2007-06-01

Patch-clamp recording has revolutionized the study of ion channels, transporters, and the electrical activity of small cells. Vital to this method is formation of a tight seal between glass recording pipette and cell membrane. To better understand seal formation and improve practical application of this technique, we examine the effects of divalent ions, protons, ionic strength, and membrane proteins on adhesion of membrane to glass and on seal resistance using both patch-clamp recording and atomic force microscopy. We find that H(+), Ca(2+), and Mg(2+) increase adhesion force between glass and membrane (lipid and cellular), decrease the time required to form a tight seal, and increase seal resistance. In the absence of H(+) (10(-10) M) and divalent cations (<10(-8) M), adhesion forces are greatly reduced and tight seals are not formed. H(+) (10(-7) M) promotes seal formation in the absence of divalent cations. A positive correlation between adhesion force and seal formation indicates that high resistance seals are associated with increased adhesion between membrane and glass. A similar ionic dependence of the adhesion of lipid membranes and cell membranes to glass indicates that lipid membranes without proteins are sufficient for the action of ions on adhesion.

Engineered glass seals for solid-oxide fuel cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Surdoval, Wayne; Lara-Curzio, Edgar; Stevenson, Jeffry

2017-02-07

A seal for a solid oxide fuel cell includes a glass matrix having glass percolation therethrough and having a glass transition temperature below 650.degree. C. A deformable second phase material is dispersed in the glass matrix. The second phase material can be a compliant material. The second phase material can be a crushable material. A solid oxide fuel cell, a precursor for forming a seal for a solid oxide fuel cell, and a method of making a seal for a solid oxide fuel cell are also disclosed.

Some developments on ceramic-to-metal and glass-ceramics-to-metal seals and related studies

NASA Astrophysics Data System (ADS)

Kothiyal, G. P.; Goswami, M.; Shrikhande, V. K.

2008-05-01

Seals and coatings based on ceramics and glass-ceramics find numerous applications in different disciplines of science and technology including space, accelerators, nuclear energy, chemical industry. Ceramic-to-metal (CM) seals based on conventional design (using brazing alloys) and glass-ceramics have been prepared. While Ag-Cu brazing alloy has been used in conventional CM seal, we have employed lithium zinc silicate (LZS) and lithium aluminum silicate (LAS) glass-ceramics for glass-ceramics-to-metal (GCM) seals. LZS glass-ceramics based on two different compositions; (a) LZSL composition (wt.%)- Li2O: 12.65, ZnO: 1.85, SiO2: 74.4, Al2O3: 3.8, K2O: 2.95, P2O5: 3.15, and B2O3: 1.2 (low ZnO) and (b) LZSH composition (wt.%)- Li2O: 8.9, ZnO: 24.03, SiO2: 53.7, Na2O: 5.42, P2O5: 2.95, and B2O3: 5.0 (high ZnO) were prepared with desired sealing characteristics for matched type seals. In addition, (wt.%) 12.6Li2O-71.7SiO2-5.1Al2O3-4.9K2O-3.2B2O3-2.5P2O5 (LAS-GC) was investigated for compressive type of seal. LZS glass-ceramics-to-Cu as well as SS-321 seals were found to withstand a vacuum of 10-6 Torr with leak rate 10-9 Torr. 1/s and LAS GC-to-SS304 seal showed high pressure endurance of 12000psi. In order to understand the mechanism of sealing, glass-ceramics-to-metal interface study has also been carried out.

A modeling study on the thermomechanical behavior of glass-ceramic and self-healing glass seals at elevated temperatures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Govindaraju, Nirmal; Liu, Wenning N.; Sun, Xin

Hermetic gas seals are critical components for planar solid oxide fuel cells. This article focuses on comparative evaluation of a glass-ceramic developed by the Pacific Northwest National Laboratory (PNNL) and a self-healing glass seal developed by the University of Cincinnati. The stress and strain levels in the Positive electrode-Electrolyte-Negative electrode (PEN) seal in one cell stack are evaluated using a multi-physics simulation package developed at PNNL. Simulations were carried out with and without consideration of clamping force and stack body force, respectively. The results indicate that the overall stress and strain levels are dominated by the thermal expansion mismatches betweenmore » the different cell components. Further, compared with glass-ceramic seal, the self-healing glass seal results in much lower steady state stress due to its much lower stiffness at the operating temperature of SOFC, and also exhibits much shorter relaxation times due to high creep rate. It is also noted that the self-healing glass seal will experience continuing creep deformation under the operating temperature of SOFC therefore resulting in possible overflow of the sealing materials. Further stopper material may need to be added to maintain its geometric stability during operation.« less

Sodium nitrate containing mixture for producing ceramic-glass-ceramic seal by microwave heating

DOEpatents

Blake, R.D.; Meek, T.T.

1984-10-10

A mixture for, and method of using such a mixture, for producing a ceramic-glass-ceramic seal by the use of microwave energy are disclosed, wherein the mixture comprises a glass sealing material, a coupling agent, and an oxidizer. The seal produced exhibits greater strength due to its different microstructure. Sodium nitrate is the most preferred oxidizer.

Flexible edge seal for vacuum insulating glazing units

DOEpatents

Bettger, Kenneth J.; Stark, David H.

2012-12-11

A flexible edge seal is provided for a vacuum insulating glazing unit having a first glass pane and a second glass pane spaced-apart from the first. The edge seal comprises a seal member formed of a hermetically bondable material and having a first end, a second end and a center section disposed therebetween. The first end is hermetically bondable to a first glass pane. The second end is hermetically bondable to a second glass pane. The center section comprises a plurality of convolutes.

Improving the chemical compatibility of sealing glass for solid oxide fuel cells: Blocking the reactive species by controlled crystallization

NASA Astrophysics Data System (ADS)

Zhang, Teng; Zou, Qi; Zeng, Fanrong; Wang, Shaorong; Tang, Dian; Yang, Hiswen

2012-10-01

The chemical compatibility of sealing glass is of great importance for Solid oxide fuel cell (SOFC). In this work, the interfacial reaction between sealing glass and Cr-containing interconnect alloy is characterized by reacting Cr2O3 powders with a representative SrO-containing glass crystallized by different heat-treatment schedules. The crystalline structure and crystalline content of sealing glass are determined by X-ray diffraction. The results show that the fraction of Cr6+ decreases from 39.8 ± 1.9% for quenched glass to 8.2 ± 0.4% for glass crystallized at 900 °C for 2 h. In addition, the interfacial reaction can be further reduced with increasing crystallization temperature and time as well as the addition of nucleation agent (TiO2). The formation of some Sr-containing crystalline phases, Sr2SiO4 and Sr(TiO3), contributes to the improvement of chemical compatibility of sealing glass, in agreement with the results of thermodynamic calculations.

Innovative Self-Healing Seals for Solid Oxide Fuel Cells (SOFC)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raj Singh

Solid oxide fuel cell (SOFC) technology is critical to several national initiatives. Solid State Energy Conversion Alliance (SECA) addresses the technology needs through its comprehensive programs on SOFC. A reliable and cost-effective seal that works at high temperatures is essential to the long-term performance of the SOFC for 40,000 hours at 800°C. Consequently, seals remain an area of highest priority for the SECA program and its industry teams. An innovative concept based on self-healing glasses was advanced and successfully demonstrated through seal tests for 3000 hours and 300 thermal cycles to minimize internal stresses under both steady state and thermalmore » transients for making reliable seals for the SECA program. The self-healing concept requires glasses with low viscosity at the SOFC operating temperature of 800°C but this requirement may lead to excessive flow of the glass in areas forming the seal. To address this challenge, a modification to glass properties by addition of particulate fillers is pursued in the project. The underlying idea is that a non-reactive ceramic particulate filler is expected to form glass-ceramic composite and increase the seal viscosity thereby increasing the creep resistance of the glass-composite seals under load. The objectives of the program are to select appropriate filler materials for making glass-composite, fabricate glass-composites, measure thermal expansion behaviors, and determine stability of the glass-composites in air and fuel environments of a SOFC. Self-healing glass-YSZ composites are further developed and tested over a longer time periods under conditions typical of the SOFCs to validate the long-term stability up to 2000 hours. The new concepts of glass-composite seals, developed and nurtured in this program, are expected to be cost-effective as these are based on conventional processing approaches and use of the inexpensive materials.« less

Method for forming glass-to-metal seals

DOEpatents

Kramer, Daniel P.; Massey, Richard T.

1986-01-01

A method for forming a glass-to-metal seal in which the glass has a higher melting point than the metal. The molten glass is vacuum injection molded onto the metal, thus melting a very thin layer of the surface of the metal long enough to form a seal, but not long enough to cause a distortion in the shape of the metal component.

Glass-to-Metal Seal Against Liquid Helium

NASA Technical Reports Server (NTRS)

Watkins, John L.; Gatewood, John R.

1987-01-01

Simple compression joint with indium gasket forms demountable seal for superfluids. Seal developed for metal lid on glass jar used in experiments on liquid helium. Glass container allows contents to be viewed for such purposes as calibration of liquid-level detectors and adjustments of displacement plungers. Seal contains liquid helium even when temperature drops below 2.19K. Made from inexpensive, commercially available materials and parts.

Numerical and Experimental Study of Transport Phenomena in Directional Solidification of Succinonitrile

NASA Technical Reports Server (NTRS)

de Groh, Henry C., III; Yao, Minwu

1994-01-01

A numerical and experimental study of the growth of succinonitrile (SCN) using a horizontal Bridginan furnace and transparent glass ampoule was conducted. Two experiments were considered: one in which the temperature profile was fixed relative to the ampoule (no-growth case); and a second in which the thermal profile was translated at a constant rate (steady growth case). Measured temperature profiles on the outer surface of the ampoule were used as thermal boundary conditions for the modelling. The apparent heat capacity formulation combined with the variable viscositymeth was used to model the phase change in SeN. Both 2-D and 3-D models were studied and numerical solutions obtained using the commercial finite element code, FIDAP1. Comparison of the numerical results to experimental data showed excellent agreement. The complex 3-D shallow-cavity flow in the melt, differences between 2-D and 3-D models, effects of natural convection on the thermal gradient and shape of the solid/liquid interface, and the sensitivity of simulations to specific assumptions, are also discussed.

Te-and Zn-Doped InSb Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Marin, C.; Volz, M.; Bonner, W. A.; Duffar, T.

2004-01-01

In 2002, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation, seven doped InSb crystals were grown in microgravity at the International Space Station. The key goals of the SUBSA investigation are: (a) to clarify the origin of the melt convection in space laboratories; (b) to reduce melt convection to the level which allows reproducible diffusion-controlled segregation; (e) to explore the submerged baffle process and liquid encapsulation in microgravity. 30 crystal growth experiments were conducted in the ground unit, to optimize the design of flight ampoules and to test the transparent SUBSA furnace developed by TecMasters Inc. The specially designed furnace, allowed observation of the crystal growth process (melting, seeding, motion of the solid-liquid interface, etc.). In the summer of 2002, eight crystal growth experiments were conducted in the Microgravity Science Glovebox (MSG) facility at the ISS. Four Te-doped (k = 0.5) and three Zn-doped (k2.9) crystals were grown on undoped seeds. In one experiment, we were not able to seed and grow. The seven grown crystals were sectioned and analyzed using SIMS. The design of the SUBSA ampoules, the segregation data and the video images obtained during the SUBSA flight experiments will be presented and discussed.

Method for forming glass-to-metal seals

DOEpatents

Kramer, D.P.; Massey, R.T.

1985-08-26

Disclosed is a method for forming a glass-to-metal seal in which the glass has a higher melting point than the metal. The molten glass is vacuum injection molded onto the metal, thus melting a very thin layer of the surface of the metal long enough to form a seal, but not long enough to cause a distortion in the shape of the metal component.

Method of processing "BPS" glass ceramic and seals made therewith

DOEpatents

Reed, Scott T.; Stone, Ronald G.; McCollister, Howard L.; Wengert, deceased, Paul R.

1998-01-01

A glass ceramic composition, a glass ceramic-to-metal seal, and more specifically a hermetic glass ceramic-to-metal seal prepared by subjecting a glass composition comprising, by weight percent, SiO.sub.2 (65-80%), LiO.sub.2 (8-16%), Al.sub.2 O.sub.3 (2-8%), K.sub.2 O (1-8%), P.sub.2 O.sub.5 (1-5%), B.sub.2 O.sub.3 (0.5-7%), and ZnO (0-5%) to the following processing steps: 1) heating the glass composition in a belt furnace to a temperature sufficient to melt the glass and crystallize lithium phosphate, 2) holding at a temperature and for a time sufficient to create cristobalite nuclei, 3) cooling at a controlled rate and to a temperature to cause crystallization of lithium silicates and growth of cristobalite, and 4) still further cooling in stages to ambient temperature. This process produces a glass ceramic whose high coefficient of thermal expansion (up to 200.times.10.sup.-7 in/in/.degree.C.) permits the fabrication of glass ceramic-to-metal seals, and particularly hermetic glass ceramic seals to nickel-based and stainless steel alloys and copper.

Method of processing ``BPS`` glass ceramic and seals made therewith

DOEpatents

Reed, S.T.; Stone, R.G.; McCollister, H.L.; Wengert, P.R.

1998-10-13

A glass ceramic composition, a glass ceramic-to-metal seal, and more specifically a hermetic glass ceramic-to-metal seal prepared by subjecting a glass composition comprising, by weight percent, SiO{sub 2} (65--80%), LiO{sub 2} (8--16%), Al{sub 2}O{sub 3} (2--8%), K{sub 2}O (1--8%), P{sub 2}O{sub 5} (1--5%), B{sub 2}O{sub 3} (0.5--7%), and ZnO (0--5%) to the following processing steps: (1) heating the glass composition in a belt furnace to a temperature sufficient to melt the glass and crystallize lithium phosphate, (2) holding at a temperature and for a time sufficient to create cristobalite nuclei, (3) cooling at a controlled rate and to a temperature to cause crystallization of lithium silicates and growth of cristobalite, and (4) still further cooling in stages to ambient temperature. This process produces a glass ceramic whose high coefficient of thermal expansion (up to 200{times}10{sup {minus}7} in/in/C) permits the fabrication of glass ceramic-to-metal seals, and particularly hermetic glass ceramic seals to nickel-based and stainless steel alloys and copper. 5 figs.

Thermophysical and structural studies on some glass-ceramics and role of nano size crystallites

NASA Astrophysics Data System (ADS)

Kothiyal, G. P.; Arvind, A.; Kumar, Rakesh; Dixit, Anupam; Sharma, Kuldeep; Goswami, Madhumita

2009-07-01

In this paper, we present some studies on structure and thermophysical properties of glass and glass-ceramics with possible bio-medical and sealing applications. The glass-ceramics prepared for bio-medical applications include phosphate as well as silico-phosphate compositions. In vitro bio-compatibility/activity of these materials is discussed. The glass-ceramics used for the sealing application are lithium aluminium silicate (LAS) and lithium zinc silicate (LZS). The phase formation and some aspects of thermophysical properties and sealing are discussed.

Sealing glasses for titanium and titanium alloys

DOEpatents

Brow, Richard K.; Watkins, Randall D.

1992-01-01

Glass compositions containing CaO, Al.sub.2 O.sub.3, B.sub.2 O.sub.3, SrO and BaO of various combinations of mole % are provided. These compositions are capable of forming stable glass-to-metal seals with titanium and titanium alloys, for use in components such as seals for battery headers.

Sealing glasses for titanium and titanium alloys

DOEpatents

Brow, R.K.; Watkins, R.D.

1988-01-21

Glass compositions containing CaO, Al/sub 2/O/sub 3/, B/sub 2/O/sub 3/, SrO and BaO of various combinations of mole % are provided. These compositions are capable of forming stable glass-to-metal seals with titanium and titanium alloys, for use in components such as seals for battery headers.

Sealing glass-ceramics with near-linear thermal strain, part III: Stress modeling of strain and strain rate matched glass-ceramic to metal seals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dai, Steve; Elisberg, Brenton; Calderone, James

Thermal mechanical stresses of glass-ceramic to stainless steel (GCtSS) seals are analyzed using finite element modeling over a temperature cycle from a set temperature (T set) 500°C to -55°C, and then back to 600°C. There are two glass-ceramics that have an identical coefficient of thermal expansion (CTE) at ~16 ppm/°C but have very different linearity of thermal strains, designated as near-linear NL16 and step-like SL16, and were formed from the same parent glass using different crystallization processes. Stress modeling reveals much higher plastic strain in the stainless steel using SL16 glass-ceramic when the GCtSS seal cools from T set. Uponmore » heating tensile stresses start to develop at the GC-SS interface before the temperature reaches T set. On the other hand, the much lower plastic deformation in stainless steel accumulated during cooling using NL16 glass-ceramic allows for radially compressive stress at the GC-SS interface to remain present when the seal is heated back to T set. Finally, the qualitative stress comparison suggests that with a better match of thermal strain rate to that of stainless steel, the NL16 glass-ceramic not only improves the hermeticity of the GCtSS seals, but would also improve the reliability of the seals exposed to high-temperature and/or high-pressure abnormal environments.« less

Sealing glass-ceramics with near-linear thermal strain, part III: Stress modeling of strain and strain rate matched glass-ceramic to metal seals

DOE PAGES

Dai, Steve; Elisberg, Brenton; Calderone, James; ...

2017-04-21

Thermal mechanical stresses of glass-ceramic to stainless steel (GCtSS) seals are analyzed using finite element modeling over a temperature cycle from a set temperature (T set) 500°C to -55°C, and then back to 600°C. There are two glass-ceramics that have an identical coefficient of thermal expansion (CTE) at ~16 ppm/°C but have very different linearity of thermal strains, designated as near-linear NL16 and step-like SL16, and were formed from the same parent glass using different crystallization processes. Stress modeling reveals much higher plastic strain in the stainless steel using SL16 glass-ceramic when the GCtSS seal cools from T set. Uponmore » heating tensile stresses start to develop at the GC-SS interface before the temperature reaches T set. On the other hand, the much lower plastic deformation in stainless steel accumulated during cooling using NL16 glass-ceramic allows for radially compressive stress at the GC-SS interface to remain present when the seal is heated back to T set. Finally, the qualitative stress comparison suggests that with a better match of thermal strain rate to that of stainless steel, the NL16 glass-ceramic not only improves the hermeticity of the GCtSS seals, but would also improve the reliability of the seals exposed to high-temperature and/or high-pressure abnormal environments.« less

Glassy composition for hermetic seals

DOEpatents

Wilder, Jr., James A.

1980-01-01

The invention relates to a glassy composition adaptable for sealing to aluminum-based alloys to form a hermetically-sealed insulator body. The composition may either be employed as a glass or, after devitrifying heat treatment, as a glass-ceramic.

Repair of through thickness corrosion/leaking defects in corroded pipelines using Fiber Reinforced Polymer overwrap

NASA Astrophysics Data System (ADS)

Nitheesh Kumar, P.; Khan, Vishwas Chandra; Balaganesan, G.; Pradhan, A. K.; Sivakumar, M. S.

2018-04-01

The present study is concerned with the repair of through thickness corrosion or leaking defects in metallic pipelines using a commercially available metallic seal and glass/epoxy composite. Pipe specimens are made with three different types of most commonly occurring through thickness corrosion/leaking defects. The metallic seal is applied over the through thickness corrosion/leaking defect and it is reinforced with glass/epoxy composite overwrap. The main objective of the metallic seal is to arrest the leak at live pressure. After reinforcing the metallic seal with glass/epoxy composite overwrap, the repaired composite wrap is able to sustain high pressures. Burst test is performed for different configurations of metallic seal and optimum configuration of metallic seal is determined. The optimum configurations of metallic seal for three different types of through thickness corrosion/leaking defects are further reinforced with glass/epoxy composite wrap and experimental failure pressure is determined by performing the burst test. An analytical model as per ISO 24817 has been developed to validate experimental results.

Effect of Nb2O5 doping on improving the thermo-mechanical stability of sealing interfaces for solid oxide fuel cells.

PubMed

Zhang, Qi; Du, Xinhang; Tan, Shengwei; Tang, Dian; Chen, Kongfa; Zhang, Teng

2017-07-13

Nb 2 O 5 is added to a borosilicate sealing system to improve the thermo-mechanical stability of the sealing interface between the glass and Fe-Cr metallic interconnect (Crofer 22APU) in solid oxide fuel cells (SOFCs). The thermo-mechanical stability of the glass/metal interface is evaluated experimentally as well as by using a finite element analysis (FEA) method. The sealing glass doped with 4 mol.% Nb 2 O 5 shows the best thermo-mechanical stability, and the sealing couple of Crofer 22APU/glass/GDC (Gd 0.2 Ce 0.8 O 1.9 ) remains intact after 50 thermal cycles. In addition, all sealing couples show good joining after being held at 750 °C for 1000 h. Moreover, the possible mechanism on the thermo-mechanical stability of sealing interface is investigated in terms of stress-based and energy-based perspectives.

Development of a low-permeability glass--ceramic to seal to molybdenum. [For long-life vacuum tubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eagan, R. J.

1975-03-01

This report describes the development of low-permeability glass-ceramics which can be sealed directly to molybdenum for the purpose of producing long-life vacuum tubes. Low permeability to helium and thermal expansion match to molybdenum are the bases upon which particular glass-ceramic compositions were selected and developed. The fabrication of tube envelopes using glass-ceramics is simplified when compared to conventional ceramic/metal tubes and these melting and sealing techniques are presented.

Application of I-structure though-glass interconnect filled with submicron gold particles to a hermetic sealing device

NASA Astrophysics Data System (ADS)

Nomura, Kazuya; Okada, Akiko; Shoji, Shuichi; Ogashiwa, Toshinori; Mizuno, Jun

2016-10-01

We propose hermetic sealing of a glass-to-glass structure with an I-structure through-glass interconnect via (TGV) filled with submicron Au particles. The top and bottom bumps and the TGV were formed by a simple filling process with a bump-patterned dry film resist. The sealing devices consisting of two glass substrates were bonded via Au interlayers. Vacuum ultraviolet irradiation in the presence of oxygen gas (VUV/O3) pretreatment was used for low-temperature Au-Au bonding at 200 °C. The bonded samples showed He leakage rates of less than 1.3  ×  10-9 Pa m3 s-1. The cross-sectional scanning electron microscope images of the fabricated I-structure TGV showed perfect adhesion between the I-structure TGV and glass substrate. These results indicate that the proposed I-structure TGV is suitable for hermetic sealing devices.

Post-experimental analysis of a solid oxide fuel cell stack using hybrid seals

NASA Astrophysics Data System (ADS)

Thomann, O.; Rautanen, M.; Himanen, O.; Tallgren, J.; Kiviaho, J.

2015-01-01

A post-experimental analysis of a SOFC stack is presented. The stack was operated for 1800 h at 700 °C with air and hydrogen and contained hybrid glass-Thermiculite 866 seals. The goal of this work was to investigate the sealing microstructure and possible corrosion during mid-term operation. It was found that hybrid seals could effectively compensate for manufacturing tolerances of cells and other components due to the compliance of the glass layer. Additionally, different interfaces were investigated for corrosion. Corrosion was not observed at two-phase interfaces such as Crofer 22 APU/glass, glass/electrolyte and glass/Thermiculite 866. The three-phase interface between Crofer 22 APU/glass/hydrogen exhibited no corrosion. Some evidence of non-systematic corrosion was found at the Crofer 22 APU/glass/air interface. The possible reasons for the corrosion are discussed. Lastly, dual exposure to humid hydrogen and air of the 0.2 mm Crofer 22 APU interconnect had no detrimental effect on the corrosion compared to air exposure. Overall the hybrid seals used in combination with the thin interconnects were found to be a promising solution due to the low leak rate and limited material interactions.

A Mechanistic-Based Healing Model for Self-Healing Glass Seals Used in Solid Oxide Fuel Cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Wei; Sun, Xin; Stephens, Elizabeth V.

The usage of self-healing glass as hermetic seals is a recent advancement in sealing technology development for the planar solid oxide fuel cells (SOFCs). Because of its capability of restoring the mechanical properties at elevated temperatures, the self-healing glass seal is expected to provide high reliability in maintaining the long-term structural integrity and functionality of SOFCs. In order to accommodate the design and to evaluate the effectiveness of such engineering seals under various thermo-mechanical operating conditions, computational modeling framework needs to be developed to accurately capture and predict the healing behavior of the glass material. In the present work, amore » mechanistic-based two-stage model was developed to study the stress and temperature-dependent crack healing of the self-healing glass materials. The model was first calibrated by experimental measurements combined with the kinetic Monte Carlo (kMC) simulation results and then implemented into the finite element analysis (FEA). The effects of various factors, i.e. stress, temperature, crack morphology, on the healing behavior of the glass were investigated and discussed.« less

Monolithic LTCC seal frame and lid

DOEpatents

Krueger, Daniel S.; Peterson, Kenneth A.; Stockdale, Dave; Duncan, James Brent; Riggs, Bristen

2016-06-21

A method for forming a monolithic seal frame and lid for use with a substrate and electronic circuitry comprises the steps of forming a mandrel from a ceramic and glass based material, forming a seal frame and lid block from a ceramic and glass based material, creating a seal frame and lid by forming a compartment and a plurality of sidewalls in the seal frame and lid block, placing the seal frame and lid on the mandrel such that the mandrel fits within the compartment, and cofiring the seal frame and lid block.

Stress analyses for the glass joints of contemporary sodium sulfur batteries

NASA Astrophysics Data System (ADS)

Jung, Keeyoung; Lee, Solki; Kim, Goun; Kim, Chang-Soo

2014-12-01

During the manufacturing and thermal cycles of advanced contemporary large sized sodium sulfur (NaS) batteries, thermally driven stresses can be applied to the glass sealing joints, which may result in catastrophic cell failure. To minimize the thermal stresses at the joints, there is a need to develop a method to properly estimate the maximum thermal stresses by varying the materials properties and shapes of the sealing area, and thereby determine the properties and shapes of sealing material at the joints. In the present study, the optimum coefficient of thermal expansion (CTE) of the glass sealant and end shape of the glass sealing area (i.e., concave, flat, and convex shapes) have been determined using the finite-element analysis (FEA) computation technique. The results showed that the CTE value of 7.8 × 10-6 K-1 with a convex end shape would have the lowest stress concentration in the vicinity of glass sealing joints for the prototype tubular NaS cell design adopted in this work.

Multilayer compressive seal for sealing in high temperature devices

DOEpatents

Chou, Yeong-Shyung [Richland, WA; Stevenson, Jeffry W [Richland, WA

2007-08-21

A mica based compressive seal has been developed exhibiting superior thermal cycle stability when compared to other compressive seals known in the art. The seal is composed of compliant glass or metal interlayers and a sealing (gasket) member layer composed of mica that is infiltrated with a glass forming material, which effectively reduces leaks within the seal. The compressive seal shows approximately a 100-fold reduction in leak rates compared with previously developed hybrid seals after from 10 to about 40 thermal cycles under a compressive stress of from 50 psi to 100 psi at temperatures in the range from 600.degree. C. to about 850.degree. C.

Mechanical and thermal characterization of a ceramic/glass composite seal for solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Dev, Bodhayan; Walter, Mark E.; Arkenberg, Gene B.; Swartz, Scott L.

2014-01-01

Solid oxide fuel cells (SOFCs) require seals that can function in harsh, elevated temperature environments. Comprehensive characterization and understanding of seals is needed for commercially viable SOFCs. The present research focuses on a novel ceramic/glass composite seal that is produced by roller compaction or tape casting of glass and ceramic powders and an organic binder. Upon heat treatment, micro-voids and surface anomalies are formed. Increased heating and cooling rates during the heat treatment resulted in more and larger voids. The first goal of the current research is to suggest an appropriate heating and cooling rate to minimize the formation of microstructural defects. After identifying an appropriate cure cycle, seals were thermally cycled and then characterized with laser dilatometry, X-ray diffraction, and sonic resonance. From these experiments the crystalline phases, thermal expansion, and elastic properties were determined. Subsequently compression testing with an acoustic emission (AE) sensor and post-test microstructural analysis were used to identify the formation of damage. By fully understanding the characteristics of this ceramic/glass composite seal, next generation seals can be fabricated for improved performance.

Viscous sealing glass compositions for solid oxide fuel cells

DOEpatents

Kim, Cheol Woon; Brow, Richard K.

2016-12-27

A sealant for forming a seal between at least two solid oxide fuel cell components wherein the sealant comprises a glass material comprising B.sub.2O.sub.3 as a principal glass former, BaO, and other components and wherein the glass material is substantially alkali-free and contains less than 30% crystalline material.

Controlling the reaction between boron-containing sealing glass and a lanthanum-containing cathode by adding Nb2O5

NASA Astrophysics Data System (ADS)

Zhao, Dandan; Fang, Lihua; Tang, Dian; Zhang, Teng

2016-09-01

In solid oxide fuel cell (SOFC) stacks, the volatile boron species present in the sealing glass often react with the lanthanum-containing cathode, degrading the activity of the cathode (this phenomenon is known as boron poisoning). In this work, we report that this detrimental reaction can be effectively reduced by doping bismuth-containing borosilicate sealing glass-ceramic with a niobium dopant. The addition of Nb2O5 not only condenses the [SiO4] structural units in the glass network, but also promotes the conversion of [BO3] to [BO4]. Moreover, the Nb2O5 dopant enhances the formation of boron-containing phases (Ca3B2O6 and CaB2Si2O8), which significantly reduces the volatility of boron compounds in the sealing glass, suppressing the formation of LaBO3 in the reaction couple between the glass and the cathode. The reported results provide a new approach to solve the problem of boron poisoning.

New Joint Sealants. Criteria, Design and Materials.

ERIC Educational Resources Information Center

Building Research Inst., Inc., Washington, DC.

Contents include--(1) sealing concrete joints, (2) sealing glass and metal joints, (3) metal and glass joint sealants from a fabricator's viewpoint, (4) a theory of adhesion for joint sealants, (5) geometry of simple joint seals under strain, (6) joint sealant specifications from a manufacturer's viewpoint, (7) joint sealant requirements from an…

The relationship between structural and optical properties of Se-Ge-As glasses

NASA Astrophysics Data System (ADS)

Ghayebloo, M.; Rezvani, M.; Tavoosi, M.

2018-05-01

In this study, the structural and optical characterization of bulk Se-Ge-As glasses has been investigated. In this regards, six different Se60Ge40-xAsx (0 ≤ x ≤ 25) glasses were prepared by conventional melt quenching technique in quartz ampoule. The produced samples were characterized using X-ray diffraction (XRD), Raman spectroscopy, differential thermal analysis (DTA), ultraviolet-visible (UV-Vis) and Fourier transform infrared (FTIR) spectroscopy. The fundamental absorption edge for all the glasses was analyzed in terms of the theory proposed by Davis and Mott. According to achieved results, fully amorphous phase can easily form in different Se-Ge-As systems. The thermal and optical characteristic of Se60Ge40-xAsx glasses shows anomalous behavior at 5 mol% of As for the glass transition temperature, transmittance, absorption edge, optical energy gap and Urbach energy. The highest glass transition temperature, transmittance, optical energy gap and Urbach energy properties were achieved in Se60Ge35As5 glass as a result of the highest connectivity of cations and anions in glass network.

Development of Certified Reference Materials for Diarrhetic Shellfish Poisoning Toxins, Part 1: Calibration Solutions.

PubMed

Beach, Daniel G; Crain, Sheila; Lewis, Nancy; LeBlanc, Patricia; Hardstaff, William R; Perez, Ruth A; Giddings, Sabrina D; Martinez-Farina, Camilo F; Stefanova, Roumiana; Burton, Ian W; Kilcoyne, Jane; Melanson, Jeremy E; Quilliam, Michael A; McCarron, Pearse

2016-09-01

Okadaic acid (OA) and its analogs dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic polyethers produced by marine dinoflagellates. These toxins accumulate in shellfish and cause diarrhetic shellfish poisoning (DSP) in humans. Regulatory testing of shellfish is essential to safeguard public health and for international trade. Certified reference materials (CRMs) play a key role in analytical monitoring programs. This paper presents an overview of the interdisciplinary work that went into the planning, production, and certification of calibration-solution CRMs for OA, DTX1, and DTX2. OA and DTX1 were isolated from large-scale algal cultures and DTX2 from naturally contaminated mussels. Toxins were isolated by a combination of extraction and chromatographic steps with processes adapted to suit the source and concentration of each toxin. New 19-epi-DSP toxin analogs were identified as minor impurities. Once OA, DTX1, and DTX2 were established to be of suitable purity, solutions were prepared and dispensed into flame-sealed glass ampoules. Certification measurements were carried out using quantitative NMR spectroscopy and LC-tandem MS. Traceability of measurements was established through certified external standards of established purity. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization, with components from the measurement, stability, and homogeneity studies being propagated into final combined uncertainties.

Thermal degradation of hexachlorobenzene in the presence of calcium oxide at 340-400 °C.

PubMed

Yin, Keqing; Gao, Xingbao; Sun, Yifei; Zheng, Lei; Wang, Wei

2013-11-01

Hexachlorobenzene (HCB) in the milligram range was co-heated with calcium oxide (CaO) powder in sealed glass ampoules at 340-400 °C. The heated samples were characterized and analyzed by Raman spectroscopy, elemental analysis, gas chromatography/mass spectrometry, ion chromatography, and thermal/optical carbon analysis. The degradation products of HCB were studied at different temperatures and heated times. The amorphous carbon was firstly quantitatively evaluated and was thought to be important fate of the C element of HCB. The yield of amorphous carbon in products increased with heating time, for samples treated for 8h at 340, 380 °C and 400 °C, the value were 17.5%, 34.8% and 50.2%, respectively. After identification of the dechlorination products, the HCB degradation on CaO at 340-400 °C was supposed to through dechlorination/polymerization pathway, which is induced by electron transfer, generate chloride ions and form high-molecular weight intermediates with significant levels of both hydrogen and chlorine, and finally form amorphous carbon. Higher temperature was beneficial for the dechlorination/polymerization efficiency. The results are helpful for clarifying the reaction mechanism for thermal degradation of chlorinated aromatics in alkaline matrices. Copyright © 2013 Elsevier Ltd. All rights reserved.

Welding/sealing glass-enclosed space in a vacuum

DOEpatents

Tracy, C.E.; Benson, D.K.

1996-02-06

A method of welding and sealing the edges of two juxtaposed glass sheets together to seal a vacuum space between the sheets comprises the steps of positioning a radiation absorbent material, such as FeO, VO{sub 2}, or NiO, between the radiation transmissive glass sheets adjacent the edges and then irradiating the absorbent material, preferably with a laser beam, through at least one of the glass sheets. Heat produced by the absorbed radiation in the absorbent material melts glass in the portions of both glass sheets that are adjacent the absorbent material, and the melted glass from both sheets flows together to create the weld when the melted glass cools and hardens. The absorbent material can be dissolved and diffused into the melted glass to the extent that it no longer absorbs enough energy to keep the glass melted, thus, with appropriate proportioning of absorbent material to source energy power and welding heat needed, the process can be made self-stopping. 8 figs.

Welding/sealing glass-enclosed space in a vacuum

DOEpatents

Tracy, C. Edwin; Benson, David K.

1996-01-01

A method of welding and sealing the edges of two juxtaposed glass sheets together to seal a vacuum space between the sheets comprises the steps of positioning a radiation absorbant material, such as FeO, VO.sub.2, or NiO, between the radiation transmissive glass sheets adjacent the edges and then irradiating the absorbant material, preferably with a laser beam, through at least one of the glass sheets. Heat produced by the absorbed radiation in the absorbant material melts glass in the portions of both glass sheets that are adjacent the absorbant material, and the melted glass from both sheets flows together to create the weld when the melted glass cools and hardens. The absorbant material can be dissolved and diffused into the melted glass to the extent that it no longer absorbs enough energy to keep the glass melted, thus, with appropriate proportioning of absorbant material to source energy power and welding heat needed, the process can be made self-stopping.

Molybdenum sealing glass-ceramic composition

DOEpatents

Eagan, Robert J.

1976-01-01

The invention relates to a glass-ceramic composition having low hydrogen and helium permeability properties, along with high fracture strength, a thermal coefficient of expansion similar to that of molybdenum, and adaptable for hermetically sealing to molybdenum at temperatures of between about 900.degree. and about 950.degree.C. to form a hermatically sealed insulator body.

High temperature storage characteristics of lithium sulfur dioxide cells

NASA Technical Reports Server (NTRS)

Watson, T.

1980-01-01

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.

Long-term evaluation of solid oxide fuel cell candidate materials in a 3-cell generic short stack fixture, Part II: sealing glass stability, microstructure and interfacial reactions.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chou, Y. S.; Stevenson, Jeffry W.; Choi, Jung-Pyung

2014-03-15

A generic solid oxide fuel cell stack test fixture was developed to evaluate candidate materials and processing methods under realistic conditions. Part I of the work addressed the stack fixture, seal system and cell performance of a 3-cell short stack tested at 800oC for 6000h. Commercial NiO-YSZ anode-supported thin YSZ electrolyte cells with LSM cathodes were used for assessment and were tested in constant current mode with dilute (~50% H2) fuel versus air. Part II of the work examined the sealing glass stability, microstructure development, interfacial reactions, and volatility issues. Part III of the work investigated the stability of Ce-(Mn,Co)more » spinel coating, AISI441 metallic interconnect, alumina coating, and cell degradation. After 6000h of testing, the refractory sealing glass YSO77 (Ba-Sr-Y-B-Si) showed desirable chemical compatibility with YSZ electrolyte in that no discernable interfacial reaction was identified, consistent with thermodynamic calculations. In addition, no glass penetration into the thin electrolyte was observed. At the aluminized AISI441 interface, the protective alumina coating appeared to be corroded by the sealing glass. Air side interactions appeared to be more severe than fuel side interactions. Metal species such as Cr, Mn, and Fe were detected in the glass, but were limited to the vicinity of the interface. No alkaline earth chromates were found at the air side. Volatility was also studied in a similar glass and weight loss in a wet reducing environment was determined. Using the steady-state volatility data, the life time (40,000h) weight loss of refractory sealing glass YSO77 was estimated to be less than 0.1 wt%.« less

Glass composition and process for sealing void spaces in electrochemical devices

DOEpatents

Meinhardt, Kerry D [Richland, WA; Kirby, Brent W [Kennewick, WA

2012-05-01

A glass foaming material and method are disclosed for filling void spaces in electrochemical devices. The glass material includes a reagent that foams at a temperature above the softening point of the glass. Expansion of the glass fills void spaces including by-pass and tolerance channels of electrochemical devices. In addition, cassette to cassette seals can also be formed while channels and other void spaces are filled, reducing the number of processing steps needed.

Effect of binder burnout on the sealing performance of glass ceramics for solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Ertugrul, Tugrul Y.; Celik, Selahattin; Mat, Mahmut D.

2013-11-01

The glass ceramics composite sealants are among few materials suitable for the solid oxide fuel cells (SOFC) due to their high operating temperatures (600 °C-850 °C). The glass ceramics chemically bond to both the metallic interconnector and the ceramic electrolyte and provide a gas tight connection. A careful and several stages manufacturing procedure is required to obtain a gas tight sealing. In this study, effects of binder burnout process on the sealing performance are investigated employing commercially available glass ceramic powders. The glass ceramic laminates are produced by mixing glass ceramic powders with the organic binders and employing a tape casting method. The laminates are sandwiched between the metallic interconnectors of an SOFC cell. The burnout and subsequent sealing quality are analyzed by measuring leakage rate and final macrostructure of sealing region. The effects of heating rate, dead weight load, solid loading, carrier gas and their flow rates are investigated. It is found that sealing quality is affected from all investigated parameters. While a slower heating rate is required for a better burnout, the mass flow rate of sweep gas must be adequate for removal of the burned gas. The leakage rate is reduced to 0.1 ml min-1 with 2 °C min-1 + 1 °C min-1 heating rate, 86.25% solid loading, 200 N dead weight load and 500 ml min-1 sweep gas flow rate.

Microstructure characteristics of vacuum glazing brazing joints using laser sealing technique

NASA Astrophysics Data System (ADS)

Liu, Sixing; Yang, Zheng; Zhang, Jianfeng; Zhang, Shanwen; Miao, Hong; Zhang, Yanjun; Zhang, Qi

2018-05-01

Two pieces of plate glass were brazed into a composite of glazing with a vacuum chamber using PbO-TiO2-SiO2-RxOy powder filler alloys to develop a new type of vacuum glazing. The brazing process was carried out by laser technology. The interface characteristics of laser brazed joints formed between plate glass and solder were investigated using optical microscope, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) techniques. The results show that the inter-diffusion of Pb/Ti/Si/O elements from the sealing solder toward the glass and O/Al/Si elements from the glass toward the solder, resulting in a reaction layer in the brazed joints. The microstructure phases of PbTiO3, AlSiO, SiO2 and PbO in the glass/solder interface were confirmed by XRD analysis. The joining of the sealing solder to the glass was realized by the reaction products like fibrous structures on interface, where the wetting layer can help improve the bonding performance and strength between the sealing solder and the plate glass during the laser brazing process.

Titanium hermetic seals

DOEpatents

Brow, Richard K.; Watkins, Randall D.

1995-07-04

Titanium is prenitrided by being heated in a nitrogen environment under conditions which give rise to the formation of a titanium-nitride surface layer on the titanium. Titanium thus prenitrided may be used in electrical components which are hermetically sealed using silicate glasses and standard glass sealing techniques. According to the method of the invention, alkali volatilization and formation of deleterious interfacial silicide are inhibited.

Titanium hermetic seals

DOEpatents

Brow, Richard K.; Watkins, Randall D.

1995-01-01

Titanium is prenitrided by being heated in a nitrogen environment under conditions which give rise to the formation of a titanium-nitride surface layer on the titanium. Titanium thus prenitrided may be used in electrical components which are hermetically sealed using silicate glasses and standard glass sealing techniques. According to the method of the invention, alkali volatilization and formation of deleterious interfacial silicide are inhibited.

Some properties of lithium aluminium silicate (LAS) glass-ceramics used in glass-ceramic to metal compressive seal for vacuum applications

NASA Astrophysics Data System (ADS)

Ananthanarayanan, A.; Kumar, R.; Bhattacharya, S.; Shrikhande, V. K.; Kothiyal, G. P.

2008-05-01

We report here the preparation of LAS glass-ceramics and some studies on their thermo-physical properties and microstructure, for compressive seals in vacuum applications. Glass of composition 12.6Li2O-71.7SiO2-5.1Al2O3-4.9K2O-3.2B2O3-2.5P2O5 was prepared by the conventional melt quench technique. Based on differential thermal analysis (DTA) data, glass samples were nucleated at 600°C for 2hr and were then crystallized at 800°C for 2-5hr. X-ray diffraction (XRD) spectra showed lithium disilicate to be the major phase. A dwell time of 3hr yielded a sample of good crystallinity. Dilatometric measurements of this sample on a thermo-mechanical analyzer (TMA) measured a thermal expansion coefficient (TEC) of 94.61×10-7°C-1. Glass transition temperature (Tg), and dilatometric softening temperature (Tds) of the sample was recorded as 585°C and 830°C respectively. Considering TEC and Tds compression type seals were prepared with SS304 (TEC = 172×10-7°C-1) housing of length 15mm, outer diameter 30mm and inner diameter 15mm. After pre-heat treatment of the metal components, sealing was carried out under a protective atmosphere of flowing Argon gas. The finished seal was tested for leak tightness on a He leak detector. The seal was capable of withstanding a vacuum of 10-6 Torr; at a leak rate of 10-9 Torr lit s-1. Scanning electron microscopy (SEM) was carried out on LAS before and after fabrication of compressive seal to elucidate the effect of compressive stress and the presence of metal near the interface. We observe a significant difference in microstructure due to compressive stresses of sealing and due to the presence of metal. Energy dispersive analysis of X-rays (EDAX) revealed no interdiffusion of species from glass-ceramic to metal or vice-versa.

Hermetic edge sealing of photovoltaic modules

NASA Astrophysics Data System (ADS)

1983-02-01

The edge sealing technique is accomplished by a combination of a chemical bond between glass and aluminum, formed by electrostatic bonding, and a metallurgical bond between aluminum and aluminum, formed by ultrasonic welding. Such a glass to metal seal promises to provide a low cost, long lifetime, highly effective hermetic seal which can protect module components from severe environments. Development of the sealing techniques and demonstration of their effectiveness by fabricating a small number of dummy modules, up to eight inches square in size, and testing them for hermeticity using helium leak testing methods are reviewed. Non-destructive test methods are investigated.

Hermetic edge sealing of photovoltaic modules

NASA Technical Reports Server (NTRS)

1983-01-01

The edge sealing technique is accomplished by a combination of a chemical bond between glass and aluminum, formed by electrostatic bonding, and a metallurgical bond between aluminum and aluminum, formed by ultrasonic welding. Such a glass to metal seal promises to provide a low cost, long lifetime, highly effective hermetic seal which can protect module components from severe environments. Development of the sealing techniques and demonstration of their effectiveness by fabricating a small number of dummy modules, up to eight inches square in size, and testing them for hermeticity using helium leak testing methods are reviewed. Non-destructive test methods are investigated.

Thermally-Activated Metal-to-Glass Bonding

NASA Technical Reports Server (NTRS)

Gallagher, B. D.

1986-01-01

Hermetic seals formed easily by use of metallo-organic film. Metallo-organic film thermally bonded to glass and soldered or welded to form hermetic seal. Film applied as ink consisting of silver neodecanoate in xylene. Relative amounts of ingredients selected to obtain desired viscosity. Material applied by printing or even by scribing with pen. Sealing technique useful in making solar-cell modules, microelectronic packages, and other hermetic silicon devices.

High expansion, lithium corrosion resistant sealing glasses

DOEpatents

Brow, Richard K.; Watkins, Randall D.

1991-01-01

Glass compositions containing CaO, Al.sub.2 O.sub.3, B.sub.2 O.sub.3, SrO and BaO in various combinations of mole % are provided. These compositions are capable of forming stable glass-to-metal seals with pin materials of 446 Stainless Steel and Alloy-52 rather than molybdenum, for use in harsh chemical environments, specifically in lithium batteries.

High expansion, lithium corrosion resistant sealing glasses

DOEpatents

Brow, R.K.; Watkins, R.D.

1991-06-04

Glass compositions containing CaO, Al[sub 2]O[sub 3], B[sub 2]O[sub 3], SrO and BaO in various combinations of mole % are provided. These compositions are capable of forming stable glass-to-metal seals with pin materials of 446 Stainless Steel and Alloy-52 rather than molybdenum, for use in harsh chemical environments, specifically in lithium batteries.

Hermetic fiber optic-to-metal connection technique

DOEpatents

Kramer, Daniel P.

1992-09-01

A glass-to-glass hermetic sealing technique is disclosed which can be used to splice lengths of glass fibers together. A solid glass preform is inserted into the cavity of a metal component which is then heated to melt the glass. An end of an optical fiber is then advanced into the molten glass and the entire structure cooled to solidify the glass in sealing engagement with the optical fiber end and the metal cavity. The surface of the re-solidified glass may be machined for mating engagement with another component to make a spliced fiber optic connection. The resultant structure has a helium leak rate of less than 1.times.10.sup.-8 cm.sup.3 /sec.

Apparatus and method for heating a material in a transparent ampoule. [crystal growth

NASA Technical Reports Server (NTRS)

Holland, L. R. (Inventor)

1983-01-01

An improved process for heating a material within a fused silica ampoule by radiation through the wall of the ampoule, while simultaneously passing a cooling gas around the ampoule is described. The radiation passes through a screen of fused silica so as to remove those components capable of directly heating the silica, therby increasing the temperature of the material within the ampoule above the strain point of the ampoule, while maintaining the exterior of the ampoule cool enough to prevent rupturing the amp.

Fluorescent discharge lamp

NASA Technical Reports Server (NTRS)

Mukai, E.; Otsuka, H.; Nomi, K.; Honmo, I.

1982-01-01

A rapidly illuminating fluorescent lamp 1,200 mm long and 32.5 mm in diameter with an interior conducting strip which is compatible with conventional fixtures and ballasts is described. The fluorescent lamp is composed of a linear glass tube, electrodes sealed at both ends, mercury and raregas sealed in the glass tube, a fluorescent substance clad on the inner walls of the glass tube, and a clad conducting strip extending the entire length of the glass tube in the axial direction on the inner surface of the tube.

Glass injuries seen in the emergency department of a South African district hospital

PubMed Central

Nzaumvila, Doudou; Kramer, Efraim B.

2015-01-01

Background The emergency department of Embhuleni Hospital frequently manages patients with glass-related injuries. This study assessed these injuries and the glass that caused them in more detail. Aim The objectives of our study included determining the type of glass causing these injuries and describing the circumstances associated with different types of glass injuries. Setting The emergency department of Embhuleni Hospital in Elukwatini, Mpumalanga province, South Africa. Methods This was a cross-sectional study with a sample size of 104 patients. Descriptive statistics were used to assess the characteristics of the glass injuries. Results Five different types of glass were reported to have caused the injuries, namely car glass (7.69%), glass ampoules (3.85%), glass bottles (82.69%), glass windows (3.85%) and street glass shards (1.92%). Glass bottle injuries were mainly caused by assaults (90.47%) and most victims were mostly young males (80.23%). The assaults occurred at alcohol-licensed premises in 65.11% of cases. These injuries occurred mostly over weekends (83.72%), between 18:00 and 04:00. The face (34.23%) and the scalp (26.84%) were the sites that were injured most often. Conclusion Assault is the most common cause of glass injuries, usually involving young men at alcohol-licensed premises. Glass injuries generally resulted in minor lacerations, with few complications (2.68%). PMID:26466399

Predicting Young’s Modulus of Glass/Ceramic Sealant for Solid Oxide Fuel Cell Considering the Combined Effects of Aging, Micro-Voids and Self-Healing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Wenning N.; Sun, Xin; Khaleel, Mohammad A.

We study the temperature dependent Young’s modulus for the glass/ceramic seal material used in Solid Oxide Fuel Cells (SOFCs). With longer heat treatment or aging time during operation, further devitrification may reduce the residual glass content in the seal material while boosting the ceramic crystalline content. In the meantime, micro-voids induced by the cooling process from the high operating temperature to room temperature can potentially degrade the mechanical properties of the glass/ceramic sealant. Upon reheating to the SOFC operating temperature, possible self-healing phenomenon may occur in the glass/ceramic sealant which can potentially restore some of its mechanical properties. A phenomenologicalmore » model is developed to model the temperature dependent Young’s modulus of glass/ceramic seal considering the combined effects of aging, micro-voids, and possible self-healing. An aging-time-dependent crystalline content model is first developed to describe the increase of the crystalline content due to the continuing devitrification under high operating temperature. A continuum damage mechanics (CDM) model is then adapted to model the effects of both cooling induced micro-voids and reheating induced self-healing. This model is applied to model the glass-ceramic G18, a candidate SOFC seal material previously developed at PNNL. Experimentally determined temperature dependent Young’s modulus is used to validate the model predictions« less

Semiconductor-to-metal phase change in MoTe2 layers (Conference Presentation)

NASA Astrophysics Data System (ADS)

Davydov, Albert V.; Krylyuk, Sergiy; Kalish, Irina; Meshi, Louisa; Beams, Ryan; Kalanyan, Berc; Sharma, Deepak K.; Beck, Megan; Bergeron, Hadallia; Hersam, Mark C.

2016-09-01

Molybdenum ditelluride (MoTe2), which can exist in a semiconducting prismatic hexagonal (2H) or a metallic distorted octahedral (1T') phases, is one of the very few materials that exhibit metal-semiconductor transition. Temperature-driven 2H - 1T' phase transition in bulk MoTe2 occurs at high temperatures (above 900 °C) and it is usually accompanied by Te loss. The latter can exacerbate the control over reversibility of the phase transition. Here, we study effects of high-temperature annealing on phase transition in MoTe2 single crystals. First, MoTe2 were grown in sealed evacuated quartz ampoules from polycrystalline MoTe2 powder in an iodine-assisted chemical vapor transport process at 1000 °C. The 2H and 1T' phases were stabilized by controlling the cooling rate after the growth. In particular, slow cooling at 10 °C/h rate yielded the 2H phase whereas the 1T' phase was stabilized by ice-water quenching. Next, the phase conversion was achieved by annealing MoTe2 single crystals in vacuum-sealed ampoules at 1000 °C with or without additional poly-MoTe2 powder followed by fast or slow cooling. Similarly to the CVT growth, slow cooling and quenching consistently produced 2H and 1T' phases, respectively, regardless of the initial MoTe2 crystal structure. We will discuss structural and optical properties of the as-grown and phase-converted MoTe2 single crystals using TEM, SEM/EDS, XRD, XPS and Raman. Electrical characteristics of two-terminal devices made from metallic 1T' and bottom-gated FETs made from 2H exfoliated crystals will also be presented.

Method for hermetic electrical connections

DOEpatents

Monroe, Saundra L [Tijeras, NM; Glass, S Jill [Albuquerque, NM; Stone, Ronnie G [Albuquerque, NM; Bond, Jamey T [Albuquerque, NM; Susan, Donald F [Albuquerque, NM

2011-12-27

A method of providing a hermetic, electrical connection between two electrical components by mating at least one metal pin in a glass-ceramic to metal seal connector to two electrical components, wherein the glass-ceramic to metal seal connector incorporates at least one metal pin encased (sealed) in a glass-ceramic material inside of a metal housing, with the glass-ceramic material made from 65-80% SiO.sub.2, 8-16% Li.sub.2O, 2-8% Al.sub.2O.sub.3, 1-5% P.sub.2O.sub.5, 1-8% K.sub.2O, 0.5-7% B.sub.2O.sub.3, and 0-5% ZnO. The connector retains hermeticity at temperatures as high as 700.degree. C. and pressures as high as 500 psi.

Method and apparatus for performing in-situ vacuum-assisted metal to glass sealing

DOEpatents

Kramer, D.P.; Massey, R.T.

1985-07-18

A method and apparatus for assembling and fusing glass to metal in a glass-metal electrical component is disclosed. The component includes a metallic shell formed with upper and lower cylindrical recesses connected together by longitudinal passages, a pair of metal rings and plural metal pins assembled to define electrical feed-throughs. The component parts are assembled on a fixture having a sleeve-like projection and a central mounting projection establishing concentric nesting surfaces to which the metal rings are slip-fitted in concentric alignment with each other spaced from sidewalls of the lower recess. The pins are in electrical contact with the metal rings. A glass pre-form is seated within the upper recess. The assembled structure is heated to a temperature sufficient to melt the glass pre-form which flows under gravity through the passages into the lower recess to provide an insulative seal between the metal parts. The gravity flow of glass is assisted by applying vacuum to the lower recess, ensuring that all spaces between the metal parts are filled with sealing glass without formation of bubbles.

Method and apparatus for performing in-situ vacuum-assisted metal to glass sealing

DOEpatents

Kramer, Daniel P.; Massey, Richard T.

1986-01-01

A method and apparatus for assembling and fusing glass to metal in a glass-metal electrical component is disclosed. The component includes a metallic shell formed with upper and lower cylindrical recesses connected together by longitudinal passages, a pair of metal rings and plural metal pins assembled to define electrical feed-throughs. The component parts are assembled on a fixture having a sleeve-like projection and a central mounting projection establishing concentric nesting surfaces to which the metal rings are slip-fitted in concentric alignment with each other spaced from sidewalls of the lower recess. The pins are in electrical contact with the metal rings. A glass pre-form is seated within the upper recess. The assembled structure is heated to a temperature sufficient to melt the glass pre-form which flows under gravity through the passages into the lower recess to provide an insulative seal between the metal parts. The gravity flow of glass is assisted by applying vacuum to the lower recess, ensuring that all spaces between the metal parts are filled with sealing glass without formation of bubbles.

The effect of heat sinks in GTA microwelding

DOE Office of Scientific and Technical Information (OSTI.GOV)

Knorovsky, G.A.; Burchett, S.N.

1989-01-01

When miniature devices containing glass-to-metal seals are closure welded it is accepted practice to incorporate thermal heat sinks into the fixturing. This is intended to assure that the heat from gas tungsten arc (GTA) welding will not cause thermal stress-induced cracking of the seals and loss of hermeticity. The design of these heat sinks has never been systematically studied; instead only ''engineering horse sense'' has been applied. This practice has been successful in the past; however, the component being GTA welded have become smaller and more complex (i.e., more pins) and glass cracking problems are being encountered. The technology ofmore » producing glass seal-containing lids (called ''headers'') has benefited from finite element analyses in deciding how to optimally dimension pin-to-glass seal diameter ratios and glass-to-metal thickness ratios in order to minimize thermal stresses locked in during manufacture. It appeared likely that an analysts of the stresses generated by welding would also be beneficial. Recently, computer speed and code capabilities have increased to the point where finite element analysis of a close simulation of real hardware can be made, including the effect of external heat sinks. The work reported here involves an analysis (with some supporting experimental data) of a miniature thermal battery which encountered glass cracking problems. In the course of the analysis various heat sink practices were examined. Among other findings, through-thickness thermal gradients in a header with a heat sink were found to equal in-plane thermal gradients in a header without any heat sinking at the glass seal positions. Also noted were significant variations due to relatively minor changes in the weld preparation geometry. A summary of good practice for heat sinking will be presented. 4 refs., 6 figs., 2 tabs.« less

Effect of aluminizing of Cr-containing ferritic alloys on the seal strength of a novel high-temperature solid oxide fuel cell sealing glass

NASA Astrophysics Data System (ADS)

Chou, Yeong-Shyung; Stevenson, Jeffry W.; Singh, Prabhakar

A novel high-temperature alkaline earth silicate sealing glass was developed for solid oxide fuel cell (SOFC) applications. The glass was used to join two metallic coupons of Cr-containing ferritic stainless steel for seal strength evaluation. In previous work, SrCrO 4 was found to form along the glass/steel interface, which led to severe strength degradation. In the present study, aluminization of the steel surface was investigated as a remedy to minimize or prevent the strontium chromate formation. Three different processes for aluminization were evaluated with Crofer22APU stainless steel: pack cementation, vapor-phase deposition, and aerosol spraying. It was found that pack cementation resulted in a rough surface with occasional cracks in the Al-diffused region. Vapor-phase deposition yielded a smoother surface, but the resulting high Al content increased the coefficient of thermal expansion (CTE), resulting in the failure of joined coupons. Aerosol spraying of an Al-containing salt resulted in the formation of a thin aluminum oxide layer without any surface damage. The room temperature seal strength was evaluated in the as-fired state and in environmentally aged conditions. In contrast to earlier results with uncoated Crofer22APU, the aluminized samples showed no strength degradation even for samples aged in air. Interfacial and chemical compatibility was also investigated. The results showed aluminization to be a viable candidate approach to minimize undesirable chromate formation between alkaline earth silicate sealing glass and Cr-containing interconnect alloys for SOFC applications.

Integral glass encapsulation for solar arrays

NASA Technical Reports Server (NTRS)

Young, P. R.

1977-01-01

Electrostatic bonding has been used to join silicon solar cells to borosilicate glass without the aid of any organic binders or adhesives. The results of this investigation have been to demonstrate, without question, the feasibility of this process as an encapsulation technique. The potential of ESB for terrestrial solar arrays was clearly shown. The process is fast, reproducible, and produces a permanent bond between glass and silicon that is stronger than the silicon itself. Since this process is a glass sealing technique requiring no organics it makes moisture tight sealing of solar cells possible.

Glass-to-metal seals comprising relatively high expansion metals

NASA Technical Reports Server (NTRS)

Hirayama, C. (Inventor)

1974-01-01

A glass suitable for glass-to-metal seals that has a resistance to attack by moisture and a high coefficient of linear thermal expansion is introduced. Linear expansion covers the range from 12 to 14 x 10 to the minus 6 C between room temperature and 500 C. The glass is essentially composed of, by molar percent, about 9% of K2O, about 10% of Na2O, about 70% of SiO2, about 6% Al2O3, and about 5% of MgO.

Planar ultra thin glass seals with optical fiber interface for monitoring tamper attacks on security eminent components

NASA Astrophysics Data System (ADS)

Thiel, M.; Flachenecker, G.; Schade, W.; Gorecki, C.; Thoma, A.; Rathje, R.

2017-11-01

Optical seals consisting of waveguide Bragg grating sensor structures in ultra thin glass transparencies have been developed to cover security relevant objects for detection of unauthorized access. For generation of optical signature in the seals, femtosecond laser pulses were used. The optical seals were connected with an optical fiber to enable external read out of the seal. Different attack scenarios for getting undetected access to the object, covered by the seal, were proven and evaluated. The results presented here, verify a very high level of security. An unauthorized detaching and subsequent replacement by original or copy of the seals for tampering would be accompanied with a very high technological effort, posing a substantial barrier towards an attacker. Additionally, environmental influences like temperature effects have a strong but reproducible influence on signature, which in context of a temperature reference database increases the level of security significantly.

Sealing glass-ceramics with near linear thermal strain, Part II: Sequence of crystallization and phase stability

DOE PAGES

Dai, Steve Xunhu; Rodriguez, Mark A.; Griego, James M.

2016-06-01

Here, the sequence of crystallization in a re-crystallizable lithium silicate sealing glass-ceramic Li 2O-SiO 2-Al 2O 3-K 2O-B 2O 3-P 2O 5-ZnO was analyzed by in situ high temperature X-ray diffraction (HTXRD). Glass-ceramic specimens have been subjected to a 2-stage heat treatment schedule, including rapid cooling from sealing temperature to a 1st hold temperature 650 °C, following by heating to a 2nd hold temperature of 810 °C. Notable growth and saturation of Quartz was observed at 650 °C (1st hold).

Ampoule Failure System

NASA Technical Reports Server (NTRS)

Watring, Dale A. (Inventor); Johnson, Martin L. (Inventor)

1996-01-01

An ampoule failure system for use in material processing furnaces comprising a containment cartridge and an ampoule failure sensor. The containment cartridge contains an ampoule of toxic material therein and is positioned within a furnace for processing. An ampoule failure probe is positioned in the containment cartridge adjacent the ampoule for detecting a potential harmful release of toxic material therefrom during processing. The failure probe is spaced a predetermined distance from the ampoule and is chemically chosen so as to undergo a timely chemical reaction with the toxic material upon the harmful release thereof. The ampoule failure system further comprises a data acquisition system which is positioned externally of the furnace and is electrically connected to the ampoule failure probe so as to form a communicating electrical circuit. The data acquisition system includes an automatic shutdown device for shutting down the furnace upon the harmful release of toxic material. It also includes a resistance measuring device for measuring the resistance of the failure probe during processing. The chemical reaction causes a step increase in resistance of the failure probe whereupon the automatic shutdown device will responsively shut down the furnace.

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

NASA Technical Reports Server (NTRS)

Thomas, Walter B., III; Lewis, Michael D.

1991-01-01

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.

Ammonia-treated phosphate glasses useful for sealing to metals metals

DOEpatents

Brow, Richard K.; Day, Delbert E.

1991-01-01

A method of improving surface-dependent properties of phosphate glass such as durability and wear resistance without significantly affecting its thermal expansion coefficient is provided which comprises annealing the glass in a dry ammonia atmosphere at temperatures approximating the transition temperature of the glass. The ammonia annealing treatment of the present invention is carried out for a time sufficient to allow incorporation of a thin layer of nitrogen into the surface of the phosphate glass, and the treatment improves the durability of the glass without the reduction in the thermal expansion coefficient that has restricted the effectiveness of prior ammonia treatments. The improved phosphate glass resulting from this method is superior in wear resistance, yet maintains suitable thermal expansion properties so that it may be used effectively in a variety of applications requiring hermetic glass-metal seals.

Ammonia-treated phosphate glasses useful for sealing to metals

DOEpatents

Brow, R.K.; Day, D.E.

1991-09-03

A method of improving surface-dependent properties of phosphate glass such as durability and wear resistance without significantly affecting its thermal expansion coefficient is provided which comprises annealing the glass in a dry ammonia atmosphere at temperatures approximating the transition temperature of the glass. The ammonia annealing treatment of the present invention is carried out for a time sufficient to allow incorporation of a thin layer of nitrogen into the surface of the phosphate glass, and the treatment improves the durability of the glass without the reduction in the thermal expansion coefficient that has restricted the effectiveness of prior ammonia treatments. The improved phosphate glass resulting from this method is superior in wear resistance, yet maintains suitable thermal expansion properties so that it may be used effectively in a variety of applications requiring hermetic glass-metal seals.

Absorption and emission spectra of Ga1.7Ge25As8.3S65 glasses doped with rare-earth ions

NASA Astrophysics Data System (ADS)

Lupan, E. V.; Iaseniuc, O. V.; Ciornea, V. I.; Iovu, M. S.

2016-12-01

Excellent optical properties of chalcogenide glasses make them interesting for optoelectronic devices in the visible (VIS) and, especially, in the near- and mid-infrared (NIR and MIR) spectral regions. The rare-earth (RE3+) doped Ga17Ge25As8.3S65 glasses were prepared in evacuated ( 10-5 Pa) silica-glass ampoules which were heated up to 1000 °C at 2-4°C min-1, and then the melt was quenched. The absorption and photoluminescence spectra in the visible and near IR regions for GA1.7Ge25As8.3S65 doped with rare-earth RE+) ions (Sm3+, Nd3+, Pr3+, Dy3+ and co-doped with Ho3++Dy3+) are investigated. The energy transfer of the absorbed light in the broad band Urbach region of the host glass to the RE3+ ions is suggested for increasing the emission efficiency. The investigated Ga17Ge25As8.3S65 glasses doped with RE3+ ions are promising materials for optical amplifiers operating at 1300 and 1500 nm telecommunication windows.

Method of Promoting Single Crystal Growth During Melt Growth of Semiconductors

NASA Technical Reports Server (NTRS)

Su, Ching-Hua (Inventor)

2013-01-01

The method of the invention promotes single crystal growth during fabrication of melt growth semiconductors. A growth ampoule and its tip have a semiconductor source material placed therein. The growth ampoule is placed in a first thermal environment that raises the temperature of the semiconductor source material to its liquidus temperature. The growth ampoule is then transitioned to a second thermal environment that causes the semiconductor source material in the growth ampoule's tip to attain a temperature that is below the semiconductor source material's solidus temperature. The growth ampoule so-transitioned is then mechanically perturbed to induce single crystal growth at the growth ampoule's tip.

Seal glass compatibility with bare and (Mn,Co) 3O 4 coated Crofer 22 APU alloy in different atmospheres

NASA Astrophysics Data System (ADS)

Mahapatra, M. K.; Lu, K.

To prevent gas mixing and leakage during solid oxide fuel/electrolyzer cell operation, the interconnect/seal glass interface should bond well and remain stable. A SrO-La 2O 3-Al 2O 3-SiO 2 (SABS-0) seal glass has been bonded to bare Crofer 22 APU alloy and (Mn,Co) 3O 4 coated Crofer 22 APU alloy. The stability of the interconnect/SABS-0 interface has been studied in air and H 2/H 2O atmospheres at 800 °C for 1000 h. The interconnect/seal glass interaction involves the oxidation of the bare and (Mn,Co) 3O 4 coated Crofer 22 APU alloy surfaces, inter-diffusion of elements, chemical reaction, and the devitrification of the SABS-0 glass. The study shows that the thermal treatment atmosphere greatly affects the interfacial stability of both bare Crofer 22 APU/SABS-0 and (Mn,Co) 3O 4 coated Crofer 22 APU/SABS-0 samples. The interfacial stability is better in the H 2/H 2O atmosphere for both samples. The instability of the (Mn,Co) 3O 4 coating under the thermal treatment conditions degrades the interfacial compatibility of the (Mn,Co) 3O 4 coated Crofer 22 APU/SABS-0 sample.

Approximal sealings on lesions in neighbouring teeth requiring operative treatment: an in vitro study.

PubMed

Cartagena, Alvaro; Bakhshandeh, Azam; Ekstrand, Kim Rud

2018-02-07

With this in vitro study we aimed to assess the possibility of precise application of sealant on accessible artificial white spot lesions (WSL) on approximal surfaces next to a tooth surface under operative treatment. A secondary aim was to evaluate whether the use of magnifying glasses improved the application precision. Fifty-six extracted premolars were selected, approximal WSL lesions were created with 15% HCl gel and standardized photographs were taken. The premolars were mounted in plaster-models in contact with a neighbouring molar with Class II/I-II restoration (Sample 1) or approximal, cavitated dentin lesion (Sample 2). The restorations or the lesion were removed, and Clinpro Sealant was placed over the WSL. Magnifying glasses were used when sealing half the study material. The sealed premolar was removed from the plaster-model and photographed. Adobe Photoshop was used to measure the size of WSL and sealed area. The degree of match between the areas was determined in Photoshop. Interclass agreement for WSL, sealed, and matched areas were found as excellent (κ = 0.98-0.99). The sealant covered 48-100% of the WSL-area (median = 93%) in Sample 1 and 68-100% of the WSL-area (median = 95%) in Sample 2. No statistical differences were observed concerning uncovered proportions of the WSL-area between groups with and without using magnifying glasses (p values ≥ .19). However, overextended sealed areas were more pronounced when magnification was used (p = .01). The precision did not differ between the samples (p = .31). It was possible to seal accessible approximal lesions with high precision. Use of magnifying glasses did not improve the precision.

Temperature sensor with improved thermal barrier and gas seal between the probe and housing

DOEpatents

O'Connell, David Peter; Sumner, Randall Christian

1998-01-01

A temperature sensor comprising: a hollow tube with a first end and a second end, wherein the second end is closed sealing a cavity within the tube from an environment outside of the tube and wherein the first end has an exterior cylindrical surface; a temperature responsive sensing element within the tube proximate to the second end; a glass cylinder having an inner cylindrical surface in sealing engagement with the exterior cylindrical surface of the first end of the tube; and a sensor housing having an inner cylindrical cavity bounded by an inner cylindrical wall, wherein an outer cylindrical surface of the glass cylinder is sealingly engaged with the inner cylindrical wall.

Ampoule failure sensor time response testing: Experiment 1

NASA Technical Reports Server (NTRS)

Johnson, M. L.; Watring, D. A.

1994-01-01

The response time of an ampoule failure sensor exposed to a liquid or vapor gallium-arsenide (GaAs) is investigated. The experimental configuration represents the sample/ampoule cartridge assembly used in NASA's Crystal Growth Furnace (CGF). The sensor is a chemical fuse made from a metal with which the semiconductor material reacts more rapidly than it does with the containing cartridge. For the III-IV compound of GaAs, a platinum metal was chosen based on the reaction of platinum and arsenic at elevated temperatures which forms a low melting eutectic. Ampoule failure is indicated by a step change in resistance of the failure sensor on the order of megohms. The sensors will increase the safety of crystal growth experiments by providing an indication that an ampoule has failed. Experimental results indicate that the response times (after a known ampoule failure) for the 0.003 and 0.010 inch ampoule failure sensors are 2.4 and 3.6 minutes, respectively. This ampoule failure sensor will be utilized in the CGF during the second United States Microgravity Laboratory Mission (USML-2) and is the subject of a NASA patent application.

Growth of InSb and InI Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Churilov, A.; Volz, M. P.; Riabov, V.; Van den Berg, L.

2015-01-01

During the past 40 years, dozens of semiconductor crystal growth experiments have been conducted in space laboratories. The subsequent analysis of the space-grown crystals revealed (i) that weak convection existed in virtually all melt-growth experiments, (ii) de-wetting significantly reduced the level of stress-induced defects, and (iii) particularly encouraging results were obtained in vapor-growth experiments. In 2002, following a decade of ground based research in growing doped Ge and GaSb crystals, a series of crystal growth experiments was performed at the ISS, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation. Te- and Zn-doped InSb crystals were grown from the melt. The specially designed furnace provided a side-view of the melt and precise seeding measurement of the growth rate. At present, under sponsorship of CASIS (Center for the Advancement of Science in Space, www.iss-casis.org), we are conducting ground-based experiments with indium mono-iodide (InI) in preparation for the "SUBSA II" ISS investigation, planned for 2017. The experiments include: i) Horizontal Bridgman (HB) growth and ii) Vapor Transport (VT) growth. Finite element modeling will also be conducted, to optimize the design of the flight ampoules, for vapor and melt growth.

Investigation of a Wedge Adhesion Test for Edge Seals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kempe, Michael; Wohlgemuth, John; Miller, David

2016-09-26

Many photovoltaic (PV) technologies have been found to be sensitive to moisture that diffuses into a PV package. Even with the use of impermeable frontsheets and backsheets, moisture can penetrate from the edges of a module. To limit this moisture ingress pathway from occurring, manufacturers often use a low permeability polyisobutylene (PIB) based edge seal filled with desiccant to further restrict moisture ingress. Moisture ingress studies have shown that these materials are capable of blocking moisture for the 25-year life of a module; but to do so, they must remain well-adhered and free of cracks. This work focuses on adaptingmore » the Boeing Wedge test for use with edge seals laminated using glass substrates as part of a strategy to assess the long-term durability of edge seals. The advantage of this method is that it duplicates the residual stresses and strains that a glass/glass module may have when the lamination process results in some residual glass bending that puts the perimeter in tension. Additionally, this method allows one to simultaneously expose the material to thermal stress, humidity, mechanical stress, and ultraviolet radiation. The disadvantage of this method generally is that we are limited by the fracture toughness of the glass substrates that the edge seal is adhered to. However, the low toughness of typical uncrosslinked or sparsely crosslinked PIB makes them suitable for this technique. We present data obtained during the development of the wedge test for use with PV edge seal materials. This includes development of the measuring techniques and evaluation of the test method with relevant materials. We find consistent data within a given experiment, along with the theoretical independence of fracture toughness measurements with wedge thickness. This indicates that the test methodology is reproducible. However, even though individual experimental sets are consistent, the reproducibility between experimental sets is poor. We believe this may be due to inconsistencies in sample history, sample batch, or small changes in sample preparation/assembly from one month to the next. Because the fracture strength of typical edge seal materials is so low, they cannot be relied upon for mechanical strength. A small stress or strain on the edge seal is capable of promoting delamination or tearing causing the edge seal to fail. Because of this, edge seals are very dependent on the processing and construction parameters in the full size PV module such that any long term evaluation of their durability must be conducted on full size modules to be accurate.« less

Electron-emission characteristics of tungsten alloys: Mee 492. [No data; plasma anode tube

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moon, H.M.

A plasma-anode tube was constructed to investigate the electron-emission characteristics for rhenium, 1% thorium tungsten, and 2% thorium tungsten. The tube consists of cathode, anode, cesium reservoir, and three probes. Inside of tube is a rough vacuum by using a Varian liquid-nitrogen-cooled cryovalve and further vacuum by using a Varian absorption pumpt to 4 X IO/sup -5/ pa. The tube was sealed off from the vacuum pump after the cesium ampoule was broken. The entire plasma-anode tube except the cesiunm reservoir was placed in a Blue M Electric Company furnace whose door had been modified to permit viewing of themore » tube.« less

Li corrosion resistant glasses for headers in ambient temperature Li batteries

DOEpatents

Hellstrom, E.E.; Watkins, R.D.

1985-10-11

Glass compositions containing 10 to 50 mol% CaO, 10 to 50 mol% Al/sub 2/O/sub 3/, 30 to 60 mol% B/sub 2/O/sub 3/, and 0 to 30 mol% MgO are provided. These compositions are capable of forming a stable glass-to-metal seal possessing electrical insulating properties for use in a lithium battery. Also provided are lithium cells containing a stainless steel body and molybdenum center pin electrically insulated by means of a seal produced according to the invention.

Temperature sensor with improved thermal barrier and gas seal between the probe and housing

DOEpatents

O`Connell, D.P.; Sumner, R.C.

1998-04-28

A temperature sensor is disclosed comprising: a hollow tube with a first end and a second end, wherein the second end is closed sealing a cavity within the tube from an environment outside of the tube and wherein the first end has an exterior cylindrical surface; a temperature responsive sensing element within the tube proximate to the second end; a glass cylinder having an inner cylindrical surface in sealing engagement with the exterior cylindrical surface of the first end of the tube; and a sensor housing having an inner cylindrical cavity bounded by an inner cylindrical wall, wherein an outer cylindrical surface of the glass cylinder is sealingly engaged with the inner cylindrical wall. 1 fig.

Heat-shrink plastic tubing seals joints in glass tubing

NASA Technical Reports Server (NTRS)

Del Duca, B.; Downey, A.

1968-01-01

Small units of standard glass apparatus held together by short lengths of transparent heat-shrinkable polyolefin tubing. The tubing is shrunk over glass O-ring type connectors having O-rings but no lubricant.

Apical and root canal space sealing abilities of resin and glass ionomer-based root canal obturation systems.

PubMed

Royer, Kinga; Liu, Xue Jun; Zhu, Qiang; Malmstrom, Hans; Ren, Yan-Fang

2013-01-01

To investigate the apical sealing ability of glass ionomer and resin-based root canal obturation systems in comparison to a conventional vertical compaction of warm guttapercha. Forty-five extracted human teeth were randomly assigned into 3 groups of 15 each: a resin-based (EndoRez), a glass ionomer-based (Activ GP), and a conventional gutta-percha plus pulp sealer obturation system (GP/EWT). Apical and root canal space sealing abilities were assessed on five cross-sections 1.0 mm apart starting from the apex. Cross-section images were analysed using a focus-variation 3D scanning microscope and unsealed space was calculated as the percentage of total root canal space occupied by voids and debris. EndoRez had significantly higher rate of apical leakage and deeper dye penetration as compared to GP/EWT and Activ GP. EndoRez group had also more voids and debris (22.5%) in the root canal spaces as compared to GP/EWT (10.5%) and Activ GP (10.8%). Apical leakages occurred not only along the root canal walls, but also along the gutta-percha cones with EndoRez as a result of significant polymerisation shrinkage of the resin sealer. Resin-based EndoRez did not form an adequate apical seal of filled root canals. Glass ionomer-based Activ GP was comparable to a vertical compaction of warm guttapercha plus EWT sealer in sealing root canal spaces.

Tamper indicating seal

DOEpatents

Romero, Juan A [Albuquerque, NM; Walker, Charles A [Albuquerque, NM; Blair, Dianna S [Albuquerque, NM; Bodmer, Connie C [Albuquerque, NM

2012-05-29

Seals have a flexible wire that can be looped through a hasp-like device. The seals include a body having a recess, a plug insertable into the recess and a snap ring for fastening the plug to the body. The plug and/or body can have access holes for inserting the wire into the recess. "Teeth" on the outer diameter and through-holes through the thickness of the snap ring allow for passing the ends of the flexible wire from the recess through the snap ring. The ends of the wire can be folded back over the snap ring and into engagement with the teeth. Assembly of the seal causes the ends of the wire to be securely fastened between the teeth of the snap ring and the sidewall of the recess. Seals can include a plug and/or body made of a frangible material such as glass, ceramic, glass-ceramic or brittle polymer.

Gigaseal Mechanics: Creep of the Gigaseal under the Action of Pressure, Adhesion, and Voltage

PubMed Central

2015-01-01

Patch clamping depends on a tight seal between the cell membrane and the glass of the pipet. Why does the seal have such high electric resistance? Why does the patch adhere so strongly to the glass? Even under the action of strong hydrostatic, adhesion, and electrical forces, it creeps at a very low velocity. To explore possible explanations, we examined two physical models for the structure of the seal zone and the adhesion forces and two respective mechanisms of patch creep and electric conductivity. There is saline between the membrane and glass in the seal, and the flow of this solution under hydrostatic pressure or electroosmosis should drag a patch. There is a second possibility: the lipid core of the membrane is liquid and should be able to flow, with the inner monolayer slipping over the outer one. Both mechanisms predict the creep velocity as a function of the properties of the seal and the membrane, the pipet geometry, and the driving force. These model predictions are compared with experimental data for azolectin liposomes with added cholesterol or proteins. It turns out that to obtain experimentally observed creep velocities, a simple viscous flow in the seal zone requires ∼10 Pa·s viscosity; it is unclear what structure might provide that because that viscosity alone severely constrains the electric resistance of the gigaseal. Possibly, it is the fluid bilayer that allows the motion. The two models provide an estimate of the adhesion energy of the membrane to the glass and membrane’s electric characteristics through the comparison between the velocities of pressure-, adhesion-, and voltage-driven creep. PMID:25295693

Inexpensive Method for Coating the Interior of Silica Growth Ampoules with Pyrolytic Boron Nitride

NASA Technical Reports Server (NTRS)

Wang, Jianbin; Regel, Liya L.; Wilcox, William R.

2003-01-01

An inexpensive method was developed for coating the interior of silica ampoules with hexagonal boron nitride. An aqueous solution of boric acid was used to coat the ampoule prior to drying in a vacuum at 200 C. This coating was converted to transparent boron nitride by heating in ammonia at 1000 C. Coated ampoules were used to achieve detached solidification of indium antimonide on earth.

Residual Gas Effects on Detached Solidification in Microgravity

NASA Technical Reports Server (NTRS)

Wilcox, William R.; Regel, Liya L.; Ramakrishnan; Kota, Arun; Anand, Gaurav

2004-01-01

Our long term goal has been to make detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Thus, the objective of the current project was to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. Our focus was on the influence of oxygen on indium antimonide on clean silica ("quartz"). The research was performed by three chemical engineering graduate students, the third of whom will complete his research in the summer of 2005. Originally, we had planned to use a sealed silica cell containing a zirconia electrochemical element to control the oxygen partial pressure. However, zirconia requires an operating temperature above the 530 C melting point of InSb and is difficult to form a gas-tight seal with silica. Thus, we decided instead to flow an oxygen-containing gas through the cell. A special apparatus was designed, built and perfected. A piece of InSb was placed on a horizontal silica plate in a quartz cell. High purity argon, helium or hydrogen-containing gas is passed continuously through the cell while the oxygen concentration in the effluent gas is measured. The shape of the resulting drop was used to determine contact angle and surface tension of Ga-doped and high purity InSb. Oxygen appeared to decrease the contact angle, and definitely did not increase it. The following section gives the background for the research. Section 2 summarizes the results obtained on Ga-doped InSb with relatively high oxygen concentrations. Section 3 describes recent improvements made to the apparatus and methods of analysis. Section 4 gives recent results for high-purity InSb at low oxygen concentrations. Final results will be obtained only this summer (2005). Each section has its own references.

Sealing ceramic material in low melting point glass

NASA Technical Reports Server (NTRS)

Moritoki, M.; Fujikawa, T.; Miyanaga, J.

1984-01-01

A structured device placed in an aerated crucible to pack ceramics molding substance that is to be processed was designed. The structure is wrapped by sealing material made of pyrex glass and graphite foil or sheet with a weight attached on top of it. The crucible is made of carbon; the ceramics material to be treated through heat intervenient press process is molding substance consisting mainly of silicon nitride.

In-Vacuum Dissociator for Atomic-Hydrogen Masers

NASA Technical Reports Server (NTRS)

Vessot, R. F.

1987-01-01

Thermal control and vacuum sealing achieved while contamination avoided. Simple, relatively inexpensive molecular-hydrogen dissociator for atomic-hydrogen masers used on Earth or in vacuum of space. No air cooling required, and absence of elastomeric O-ring seals prevents contamination. In-vacuum dissociator for atomic hydrogen masers, hydrogen gas in glass dissociator dissociated by radio-frequency signal transmitted from surrounding 3-turn coil. Heat in glass conducted away by contacting metal surfaces.

Behavior of Aging, Micro-Void, and Self-Healing of Glass/Ceramic Materials and Its Effect on Mechanical Properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Wenning N.; Sun, Xin; Khaleel, Mohammad A.

This chapter first describes tests to investigate the temporal evolution of the volume fraction of ceramic phases, the evolution of micro-damage, and the self-healing behavior of the glass ceramic sealant used in SOFCs, then a phenomenological model based on mechanical analogs is developed to describe the temperature dependent Young’s modulus of glass ceramic seal materials. It was found that after the initial sintering process, further crystallization of the glass ceramic sealant does not stop, but slows down and reduces the residual glass content while boosting the ceramic crystalline content. Under the long-term operating environment, distinct fibrous and needle-like crystals inmore » the amorphous phase disappeared, and smeared/diffused phase boundaries between the glass phase and ceramic phase were observed. Meanwhile, the micro-damage was induced by the cooling-down process from the operating temperature to the room temperature, which can potentially degrade the mechanical properties of the glass/ceramic sealant. The glass/ceramic sealant self-healed upon reheating to the SOFC operating temperature, which can restore the mechanical performance of the glass/ceramic sealant. The phenomenological model developed here includes the effects of continuing aging and devitrification on the ceramic phase volume fraction and the resulted mechanical properties of glass ceramic seal material are considered. The effects of micro-voids and self-healing are also considered using a continuum damage mechanics (CDM) model. The formulation is for glass/ceramic seal in general, and it can be further developed to account for effects of various processing parameters. This model was applied to G18, and the temperature-dependent experimental measurements were used to calibrate the modeling parameters and to validate the model prediction.« less

MECHANICAL PROPERTY CHARACTERIZATIONS AND PERFORMANCE MODELING OF SOFC SEALS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koeppel, Brian J.; Vetrano, John S.; Nguyen, Ba Nghiep

2008-03-26

This study provides modeling tools for the design of reliable seals for SOFC stacks. The work consists of 1) experimental testing to determine fundamental properties of SOFC sealing materials, and 2) numerical modeling of stacks and sealing systems. The material tests capture relevant temperature-dependent physical and mechanical data needed by the analytical models such as thermal expansion, strength, fracture toughness, and relaxation behavior for glass-ceramic seals and other materials. Testing has been performed on both homogenous specimens and multiple material assemblies to investigate the effect of interfacial reactions. A viscoelastic continuum damage model for a glass-ceramic seal was developed tomore » capture the nonlinear behavior of this material at high temperatures. This model was implemented in the MSC MARC finite element code and was used for a detailed analysis of a planar SOFC stack under thermal cycling conditions. Realistic thermal loads for the stack were obtained using PNNL’s in-house multiphysics solver. The accumulated seal damage and component stresses were evaluated for multiple thermal loading cycles, and regions of high seal damage susceptible to cracking were identified. Selected test results, numerical model development, and analysis results will be presented.« less

Joining of thin glass with semiconductors by ultra-fast high-repetition laser welding

NASA Astrophysics Data System (ADS)

Horn, Alexander; Mingaeev, Ilja; Werth, Alexander; Kachel, Martin

2008-02-01

Lighting applications like OLED or on silicon for electro-optical applications need a reproducible sealing process. The joining has to be strong, the permeability for gasses and humidity very low and the process itself has to be very localized not affecting any organic or electronic parts inside the sealed region. The actual sealing process using glue does not fulfil these industrial needs. A new joining process using ultra-fast laser radiation offers a very precise joining with geometry dimensions smaller than 50 μm. Ultra-fast laser radiation is absorbed by multi-photon absorption in the glass. Due to the very definite threshold for melting and ablation the process of localized heating can be controlled without cracking. Repeating the irradiation at times smaller than the heat diffusion time the temperature in the focus is increased by heat accumulation reaching melting of the glass. Mowing the substrate relatively to the laser beam generates a seal of re-solidified glass. Joining of glass is achieved by positioning the laser focus at the interface. A similar approach is used for glass-silicon joining. The investigations presented will demonstrate the joining geometry by microscopy of cross-sections achieved by welding two glass plates (Schott D263 and AF45) with focused IR femtosecond laser radiation (wavelength λ = 1045nm, repetition rate f = 1 MHz, pulse duration t p = 500 fs, focus diameter w 0 = 4 μm, feeding velocity v= 1-10 mm/s). The strength of the welding seam is measured by tensile stress measurements and the gas and humidity is detected. A new diagnostic method for the on-line detection of the welding seam properties will be presented. Using a non-interferometric technique by quantitative phase microscopy the refractive index is measured during welding of glass in the time regime 0-2 μs. By calibration of the measured refractive index with a relation between refractive index and temperature a online-temperature detection can be achieved.

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

NASA Technical Reports Server (NTRS)

Hassan, Razi A.

1991-01-01

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.

Plastic-Sealed Hybrid Power Circuit Package

NASA Technical Reports Server (NTRS)

Miller, W. N.; Gray, O. E.

1983-01-01

Proposed design for hybrid high-voltage power-circuit package uses molded plastic for hermetic sealing instead of glass-to-metal seal. New package used to house high-voltage regulators and solid-state switches for applications in aircraft, electric automobiles, industrial equipment, satellites, solarcell arrays, and other equipment in extreme environments.

To direct the Librarian of Congress to obtain a stained glass panel depicting the seal of the District of Columbia and install the panel among the stained glass panels depicting the seals of States which overlook the Main Reading Room of the Library of Congress Thomas Jefferson Building.

THOMAS, 113th Congress

Rep. Norton, Eleanor Holmes [D-DC-At Large

2014-02-27

House - 02/28/2014 Referred to the Subcommittee on Economic Development, Public Buildings and Emergency Management. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:

Basic Research on Oxynitride Glasses.

DTIC Science & Technology

1982-07-01

The upsurge in interest in these glasses was originally motivated by their relevance to the processing of Si 3 1 4 -based ceramics (4, 5) when it was...are suggested by results obtained so far, among them refractory glass - ceramics , leach-resistant glasses , hardened optical windows, and Joining...compositions for ceramic - ceramic seals. Oxynitride Glass Synthesis The preparation of oxynitride glasses is more complex than preparation of conventional

Microgravity Disturbance Characterization of the Quench Module Insert (QMI) Phase Change Device (PCD)

NASA Technical Reports Server (NTRS)

Gattis, Christy; Rodriguez, Pete (Technical Monitor)

2000-01-01

The Materials Science Research Facility (MSRF) is a multi-user, multi-purpose facility for materials science research. One experiment within the MSRF will be the Quench Module Insert (QMI), a high-temperature furnace with unique capabilities for processing different classes of materials. The primary functions of the QMI furnace are to melt, directionally solidify, and quench metallic samples, providing data to aid in understanding the effects of the microgravity environment on the characteristics of these processed metals. The QMI houses sealed individual sample ampoules containing material to be processed. Quenching of the samples in the QMI furnace is accomplished by releasing low-melting-point metallic shoes into contact with the outside of the sample ampoule, dissipating heat and cooling the sample inside. The impact from this method of quench will induce sample vibrations which could be large enough to adversely affect sample quality. Utilizing breadboard hardware, the sample quench sequence, releasing the shoes, was conducted. Data was collected from accelerometers located on the breadboard sample cartridge, indicating the maximum acceleration achieved by the sample. The primary objective of the test described in this presentation was to determine the acceleration imparted on the sample by the shoe contact. From this information, the science community can better assess whether this method of quench will allow them to obtain the data they need.

Exploring growth conditions and Eu2+ concentration effects for KSr2I5:Eu scintillator crystals II: Ø 25 mm crystals

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Johnson, J.; Koschan, M.; Wu, Y.; Donnald, S.; Vaigneur, K.; Lukosi, E.; Melcher, C. L.

2018-02-01

Europium doped potassium strontium iodide is a very promising scintillator for national security applications due to its ease of growth and excellent scintillation properties. For this work the fast crystal growth and scintillation properties of 1-inch diameter single crystals of KSr2I5:Eu2+ (KSI:Eu) were investigated. We focused our efforts on optimizing the growth parameters required to produce one-inch diameter crystals without decreasing the previously reported fast pulling rate of 5 mm/h. Cracking was minimized by replacing the quartz ampoules with carbon coated quartz ampoules; thus, several crack free single crystals of KSI with varying Eu2+ concentrations were grown, including a Ø 1″ by 6″ long boule with 2.5% Eu. The maximum achievable performance of each crystal was measured using small 0.012 cm3 specimens. The volumetric dependencies of the light yield, energy resolution and decay time were evaluated using KSI:Eu 2% specimens with volumes ranging from 0.012 cm3 to 18 cm3. For large volumes (≥ 9 cm3), the performance was comparable to other high performing scintillators, with light yields up to 78,200 ph/MeV and energy resolutions as good as 3.2% at 662 keV. The initial version of a hermetic package has been developed, and the stability of the sealed crystal is promising.

Detached Melt and Vapor Growth of InI in SUBSA Furnace

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Riabov, V.; Volz, M. P.; van den Berg, L.; Croll, A.

2017-01-01

Indium iodide (InI) is a promising wide energy band gap nuclear detector material. It is ideal for space experiments because it is non-toxic and has a relatively low melting point of only 351 degrees Centigrade. However, it has been established that melt-grown crystals contain a large amount of second phase inclusions/precipitates. The typical size of inclusions are 1 to 27 microns in diameter, while the volume fraction of all sizes is 300 to 600 parts per million. The SEM-EDS (Scanning Electron Microscopy / Energy Dispersive X-Ray Spectroscopy) analysis of the inclusions has revealed that they all contain oxygen and some contain carbon. At present, under sponsorship of NASA and CASIS (Center for the Advancement of Science in Space), we are conducting ground-based experiments with InI in preparation for the flight experiments to be conducted in the SUBSA (Solidification Using a Baffle in Sealed Ampoules) furnace in the Microgravity Science Glovebox at the International Space Station, planned for the summer/fall of 2017. Earth-based experiments include melt and vapor growth conducted in the SUBSA ground unit, measurements of the volumetric expansion coefficient of the melt, and measurements of the wetting angle of molten InI. Finite element modeling has been conducted to optimize the design of the flight ampoules. Alloying with Tl and Ga has given promising results.

A NaI(Tl) 241Am light pulser of increased reliability by eliminating epoxy sealing

NASA Astrophysics Data System (ADS)

Kobayashi, Masaaki; Takano, Shuichi; Matsumoto, Yoshikazu

1984-07-01

A new type of NaI(Tl) 241Am light pulser has been developed without any epoxy sealing so as to improve the reliability significantly. Glass-metal fusing and metal-to-metal welding are employed to seal the NaI(Tl) crystals against moisture.

Glass-ceramic material and method of making

DOEpatents

Meinhardt, Kerry D [Richland, WA; Vienna, John D [West Richland, WA; Armstrong, Timothy R [Pasco, WA; Pederson, Larry R [Kennewick, WA

2002-08-13

The present invention is a glass-ceramic material and method of making useful for joining at least two solid ceramic parts. The seal is a blend of M.sub.A O--M.sub.B O.sub.y --SiO.sub.2 that substantially matches a coefficient of thermal expansion of the solid electrolyte. According to the present invention, a series of glass ceramics in the M.sub.A O--M.sub.B O.sub.y --SiO.sub.2 system can be used to join or seal both tubular and planar ceramic solid oxide fuel cells, oxygen electrolyzers, and membrane reactors for the production of syngas, commodity chemicals and other products.

Neutron guide

DOEpatents

Greene, Geoffrey L.

1999-01-01

A neutron guide in which lengths of cylindrical glass tubing have rectangular glass plates properly dimensioned to allow insertion into the cylindrical glass tubing so that a sealed geometrically precise polygonal cross-section is formed in the cylindrical glass tubing. The neutron guide provides easier alignment between adjacent sections than do the neutron guides of the prior art.

Sealing glass-ceramics with near-linear thermal strain, Part II: Sequence of crystallization and phase stability

DOE PAGES

Rodriguez, Mark A.; Griego, James J. M.; Dai, Steve

2016-08-22

The sequence of crystallization in a recrystallizable lithium silicate sealing glass-ceramic Li 2O–SiO 2–Al 2O 3–K 2O–B 2O 3–P 2O 5–ZnO was analyzed by in situ high-temperature X-ray diffraction (HTXRD). Glass-ceramic specimens have been subjected to a two-stage heat-treatment schedule, including rapid cooling from sealing temperature to a first hold temperature 650°C, followed by heating to a second hold temperature of 810°C. Notable growth and saturation of Quartz was observed at 650°C (first hold). Cristobalite crystallized at the second hold temperature of 810°C, growing from the residual glass rather than converting from the Quartz. The coexistence of quartz and cristobalitemore » resulted in a glass-ceramic having a near-linear thermal strain, as opposed to the highly nonlinear glass-ceramic where the cristobalite is the dominant silica crystalline phase. HTXRD was also performed to analyze the inversion and phase stability of the two types of fully crystallized glass-ceramics. While the inversion in cristobalite resembles the character of a first-order displacive phase transformation, i.e., step changes in lattice parameters and thermal hysteresis in the transition temperature, the inversion in quartz appears more diffuse and occurs over a much broader temperature range. Furthermore, localized tensile stresses on quartz and possible solid-solution effects have been attributed to the transition behavior of quartz crystals embedded in the glass-ceramics.« less

Automated method for determining Instron Residual Seal Force of glass vial/rubber closure systems. Part II. 13 mm vials.

PubMed

Ludwig, J D; Davis, C W

1995-01-01

Instron Residual Seal Force (IRSF) of 13 mm glass vial/rubber closure systems was determined using an Instron 4501 Materials Testing System and computerized data analysis. A series of three cap anvils varying in shape and dimensions were machined to optimize cap anvil performance. Cap anvils with spherical top surfaces and narrow internal dimensions produced uniform stress-deformation curves from which precise IRSF values were derived.

Preliminary thermoluminescence investigation of commercial pharmaceutical glass containers towards the sterilization dosimetry of liquid drugs.

PubMed

Kazakis, Nikolaos A; Tsirliganis, Nestor C; Kitis, George

2015-11-01

Drug sterilization with ionizing radiation is a well-established technology, which is constantly extending to several products due to its numerous advantages, since it allows the heat-free sterilization of heat-sensitive pharmaceutical preparations. In a previous study, the possibility to identify irradiated solid-state drugs by means of OSL and TL was examined with very promising findings. In the same respect, the present work aims, for the first time to the authors' best knowledge, to explore whether TL can be employed as a method for post-sterilization dosimetry on commercial liquid-state drugs, by studying the properties of their glass containers. Two different types of glass containers (bottle and ampoule) of two widely used liquid drugs, i.e., Hexalen® and Voltaren®, are used for this purpose. Both glass containers exhibit a linear TL dose response for doses up to 6kGy with a stable behavior through time, while no significant sensitization of the main peaks is observed. Thus, preliminary findings are very promising towards the post-sterilization dosimetry of liquid drugs and the use of the containers of commercial liquid drugs for normal and/or accidental dosimetry. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fifth International Standard for Gas-Gangrene Antitoxin (Perfringens) (Clostridium welchii Type A Antitoxin)

PubMed Central

Evans, D. G.; Perkins, F. T.

1963-01-01

The Fifth International Standard Gas-Gangrene Antitoxin (Perfringens) (Clostridium welchii Type A Antitoxin) was prepared from serum from immunized horses. It was freeze-dried in ampoules each containing 1 ml. Seven laboratories collaborated in assaying its potency in terms of the Fourth International Standard by the intravenous inoculation of mice. The geometric mean value, taking the results of all the laboratories, was 270 International Units per ampoule and the maximum variation between laboratories was 15%. In vitro (lecithinase) tests were also done by three laboratories, giving an average of 261 International Units per ampoule. The dry weight contents of ampoules, determined in three laboratories, varied by less than 3%, with an average of 90.35 mg per ampoule. The standard was stable for 120 hours at 56°C. Each ampoule of the Fifth International Standard for Gas-Gangrene Antitoxin (Perfringens) contains 270 International Units, and one International Unit is contained in 0.3346 mg of the International Standard. PMID:14107745

Hermetic edge sealing of photovoltaic modules

NASA Astrophysics Data System (ADS)

Nowlan, M. J.

1983-07-01

The feasibility of using an electrostatic bonding (ESB) and ultrasonic welding process to produce hermetic edge seals on terrestrial solar cell modules was investigated. The fabrication sequence is to attach an aluminum foil "gasket' to the perimeter of a glass sheet. A cell circuit is next encapsulated inside the gasket, and its aluminum foil back cover is seam welded ultrasonically to the gasket. An ESB process for sealing aluminum to glass was developed in an ambient air atmosphere, which eliminates the requirement for a vacuum or pressure vessel. An ultrasonic seam welding process was also developed which did not degrade the quality of the ESB seal. Good quality welds with minimal deformation were produced. The effectiveness of the above described sealing techniques was tested by constructing 400 sq cm (8 x 8 s64 sq in) sample modules, and then subjecting them to nondestructive fine and gross leak tests. The gross leak tests identified several different causes of leaks which were then eliminated by modifying the assembly process.

Hermetic edge sealing of photovoltaic modules

NASA Technical Reports Server (NTRS)

Nowlan, M. J.

1983-01-01

The feasibility of using an electrostatic bonding (ESB) and ultrasonic welding process to produce hermetic edge seals on terrestrial solar cell modules was investigated. The fabrication sequence is to attach an aluminum foil "gasket' to the perimeter of a glass sheet. A cell circuit is next encapsulated inside the gasket, and its aluminum foil back cover is seam welded ultrasonically to the gasket. An ESB process for sealing aluminum to glass was developed in an ambient air atmosphere, which eliminates the requirement for a vacuum or pressure vessel. An ultrasonic seam welding process was also developed which did not degrade the quality of the ESB seal. Good quality welds with minimal deformation were produced. The effectiveness of the above described sealing techniques was tested by constructing 400 sq cm (8 x 8 s64 sq in) sample modules, and then subjecting them to nondestructive fine and gross leak tests. The gross leak tests identified several different causes of leaks which were then eliminated by modifying the assembly process.

Residual Gases in Crystal Growth Systems: Their Origin, Magnitude, and Dependence on the Processing Conditions

NASA Technical Reports Server (NTRS)

Palosz, W.

2003-01-01

Residual gases present in closed ampoules may affect different crystal growth processes. Their presence may affect techniques requiring low pressures and affect the crystal quality in different ways. For that reason a good understanding and control of formation of residual gases may be important for an optimum design and meaningful interpretation of crystal growth experiments. Our extensive experimental and theoretical study includes degassing of silica glass and generation of gases from various source materials. Different materials processing conditions, like outgassing under vacuum, annealing in hydrogen, resublimation, different material preparation procedures, multiple annealings, different processing times, and others were applied and their effect on the amount and composition of gas were analyzed. The experimental results were interpreted based on theoretical calculations on diffusion in silica glass and source materials and thermochemistry of the system. Procedures for a reduction of the amount of gas are also discussed.

On the Nonlinear Behavior of a Glass-Ceramic Seal and its Application in Planar SOFC Systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nguyen, Ba Nghiep; Koeppel, Brian J.; Vetrano, John S.

2006-06-01

This paper studies the nonlinear behavior of a glass-ceramic seal used in planar solid oxide fuel cells (SOFCs). To this end, a viscoelastic damage model has been developed that can capture the nonlinear material response due to both progressive damage in the glass-ceramic material and viscous flow of the residual glass in this material. The model has been implemented in the MSC MARC finite element code, and its validation has been carried out using the experimental relaxation test data obtained for this material at 700oC, 750oC, and 800oC. Finally, it has been applied to the simulation of a SOFC stackmore » under thermal cycling conditions. The areas of potential damage have been predicted.« less

Glass/Ceramic Composites for Sealing Solid Oxide Fuel Cells

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Choi, Sung R.

2007-01-01

A family of glass/ceramic composite materials has been investigated for use as sealants in planar solid oxide fuel cells. These materials are modified versions of a barium calcium aluminosilicate glass developed previously for the same purpose. The composition of the glass in mole percentages is 35BaO + 15CaO + 5Al2O3 + 10B2O3 + 35SiO2. The glass seal was found to be susceptible to cracking during thermal cycling of the fuel cells. The goal in formulating the glass/ ceramic composite materials was to (1) retain the physical and chemical advantages that led to the prior selection of the barium calcium aluminosilicate glass as the sealant while (2) increasing strength and fracture toughness so as to reduce the tendency toward cracking. Each of the composite formulations consists of the glass plus either of two ceramic reinforcements in a proportion between 0 and 30 mole percent. One of the ceramic reinforcements consists of alumina platelets; the other one consists of particles of yttria-stabilized zirconia wherein the yttria content is 3 mole percent (3YSZ). In preparation for experiments, panels of the glass/ceramic composites were hot-pressed and machined into test bars.

Crack Growth Properties of Sealing Glasses

NASA Technical Reports Server (NTRS)

Salem, Jonathan A.; Tandon, R.

2008-01-01

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.

Hermetic Glass-To-Metal Seal For Instrumentation Window

NASA Technical Reports Server (NTRS)

Hill, Arthur J.

1992-01-01

Proposed mounting scheme for optical element of instrumentation window in pressure vessel ensures truly hermetic seal while minimizing transmission of stress to optical element. Brazed metal seal superior to conventional gaskets of elastomer, carbon, asbestos, or other material compressed between optical element and wall of vessel. Concentric brazed joints in proposed seal bond metal ring to wall of vessel and to optical element. U-shaped cross section allows ring to flex under pressure.

Development of a nondestructive leak testing method utilizing the head space analyzer for ampoule products containing ethanol-based solutions.

PubMed

Sudo, Hirotaka; O'driscoll, Michael; Nishiwaki, Kenji; Kawamoto, Yuji; Gammell, Philip; Schramm, Gerhard; Wertli, Toni; Prinz, Heino; Mori, Atsuhide; Sako, Kazuhiro

2012-01-01

The application of a head space analyzer for oxygen concentration was examined to develop a novel ampoule leak test method. Studies using ampoules filled with ethanol-based solution and with nitrogen in the headspace demonstrated that the head space analysis (HSA) method showed sufficient sensitivity in detecting an ampoule crack. The proposed method is the use of HSA in conjunction with the pretreatment of an overpressurising process known as bombing to facilitate the oxygen flow through the crack in the ampoule. The method was examined in comparative studies with a conventional dye ingress method, and the results showed that the HSA method exhibits sensitivity superior to the dye method. The results indicate that the HSA method in combination with the bombing treatment provides potential application as a leak test for the detection of container defects not only for ampoule products with ethanol-based solutions, but also for testing lyophilized products in vials with nitrogen in the head space. The application of a head space analyzer for oxygen concentration was examined to develop a novel ampoule leak test method. The proposed method is the use of head space analysis (HSA) in conjunction with the pretreatment of an overpressurising process known as bombing to facilitate oxygen flow through the crack in the ampoule for use in routine production. The result of the comparative study with a conventional dye leak test method indicates that the HSA method in combination with the bombing treatment can be used as a leak test method, enabling detection of container defects.

Quality assurance and quality control in light stable isotope laboratories: A case study of Rio Grande, Texas, water samples

USGS Publications Warehouse

Coplen, T.B.; Qi, H.

2009-01-01

New isotope laboratories can achieve the goal of reporting the same isotopic composition within analytical uncertainty for the same material analysed decades apart by (1) writing their own acceptance testing procedures and putting them into their mass spectrometric or laser-based isotope-ratio equipment procurement contract, (2) requiring a manufacturer to demonstrate acceptable performance using all sample ports provided with the instrumentation, (3) for each medium to be analysed, prepare two local reference materials substantially different in isotopic composition to encompass the range in isotopic composition expected in the laboratory and calibrated them with isotopic reference materials available from the International Atomic Energy Agency (IAEA) or the US National Institute of Standards and Technology (NIST), (4) using the optimum storage containers (for water samples, sealing in glass ampoules that are sterilised after sealing is satisfactory), (5) interspersing among sample unknowns local laboratory isotopic reference materials daily (internationally distributed isotopic reference materials can be ordered at three-year intervals, and can be used for elemental analyser analyses and other analyses that consume less than 1 mg of material) - this process applies to H, C, N, O, and S isotope ratios, (6) calculating isotopic compositions of unknowns by normalising isotopic data to that of local reference materials, which have been calibrated to internationally distributed isotopic reference materials, (7) reporting results on scales normalised to internationally distributed isotopic reference materials (where they are available) and providing to sample submitters the isotopic compositions of internationally distributed isotopic reference materials of the same substance had they been analysed with unknowns, (8) providing an audit trail in the laboratory for analytical results - this trail commonly will be in electronic format and might include a laboratory information management system, (9) making at regular intervals a complete backup of laboratory analytical data (both of samples logged into the laboratory and of mass spectrometric analyses), being sure to store one copy of this backup offsite, and (10) participating in interlaboratory comparison exercises sponsored by the IAEA and other agencies at regular intervals. ?? Taylor & Francis.

Solid Oxide Fuel Cell Seal Glass - BN Nanotubes Composites

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Choi, Sung R.; Hurst, Janet B.; Garg, Anita

2005-01-01

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.

Method for sealing an oxygen transport membrane assembly

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gonzalez, Javier E.; Grant, Arthur F.

An improved method of sealing a ceramic part to a solid part made of ceramic, metal, cermet or a ceramic coated metal is provided. The improved method includes placing a bond agent comprising an Al 2O 3 and SiO 2 based glass-ceramic material and organic binder material on adjoining surfaces of the ceramic part and the solid part. The assembly is heated to a first target temperature that removes or dissolves the organic binder material from the bond agent and the assembly is subjected to a second induction heating step at a temperature ramp rate of between about 100.degree. C.more » and 200.degree. C. per minute to temperatures where the glass-ceramic material flows and wets the interface between adjoining surfaces. The assembly is rapidly cooled at a cooling rate of about 140.degree. C. per minute or more to induce nucleation and re-crystallization of the glass-ceramic material to form a dense, durable and gas-tight seal.« less

Liquid-hydrogen/nuclear-radiation resistant seals

NASA Technical Reports Server (NTRS)

Van Auken, R.

1971-01-01

Seal employs aromatic heterocyclic polymer, polyquinoxaline, and features resin starved laminate consisting of alternate layers of woven glass fabric and polymer film. Design gives gasket a mechanical spring characteristic, eliminating cold flow and resulting in elastic recovery when gasket is unloaded.

Glass-ceramic composition for hermetic seals

DOEpatents

Ballard, Jr., Clifford P.

1979-01-01

The invention relates to a glass-ceramic composition having a high fracture strength adaptable for hermetically sealing to chromium bearing iron or nickel base alloys at temperatures of between about 950.degree. C to about 1100.degree. C to form a hermetically sealed insulator body, comprising from about 55 to about 65 weight percent SiO.sub.2, from about 0 to about 5 weight percent Al.sub.2 O.sub.3, from about 6 to about 11 weight % Li.sub.2 O, from about 25 to about 32 weight percent BaO, from about 0.5 to about 1.0 weight percent CoO and from about 1.5 to about 3.5 weight percent P.sub.2 O.sub.5.

Glass/BNNT Composite for Sealing Solid Oxide Fuel Cells

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Hurst, Janet B.; Choi, Sung R.

2007-01-01

A material consisting of a barium calcium aluminosilicate glass reinforced with 4 weight percent of boron nitride nanotubes (BNNTs) has shown promise for use as a sealant in planar solid oxide fuel cells (SOFCs).

Barium oxide, calcium oxide, magnesia, and alkali oxide free glass

DOEpatents

Lu, Peizhen Kathy; Mahapatra, Manoj Kumar

2013-09-24

A glass composition consisting essentially of about 10-45 mole percent of SrO; about 35-75 mole percent SiO.sub.2; one or more compounds from the group of compounds consisting of La.sub.2O.sub.3, Al.sub.2O.sub.3, B.sub.2O.sub.3, and Ni; the La.sub.2O.sub.3 less than about 20 mole percent; the Al.sub.2O.sub.3 less than about 25 mole percent; the B.sub.2O.sub.3 less than about 15 mole percent; and the Ni less than about 5 mole percent. Preferably, the glass is substantially free of barium oxide, calcium oxide, magnesia, and alkali oxide. Preferably, the glass is used as a seal in a solid oxide fuel/electrolyzer cell (SOFC) stack. The SOFC stack comprises a plurality of SOFCs connected by one or more interconnect and manifold materials and sealed by the glass. Preferably, each SOFC comprises an anode, a cathode, and a solid electrolyte.

Sealed glass coating of high temperature ceramic superconductors

DOEpatents

Wu, W.; Chu, C.Y.; Goretta, K.C.; Routbort, J.L.

1995-05-02

A method and article of manufacture of a lead oxide based glass coating on a high temperature superconductor is disclosed. The method includes preparing a dispersion of glass powders in a solution, applying the dispersion to the superconductor, drying the dispersion before applying another coating and heating the glass powder dispersion at temperatures below oxygen diffusion onset and above the glass melting point to form a continuous glass coating on the superconductor to establish compressive stresses which enhance the fracture strength of the superconductor. 8 figs.

Sealed glass coating of high temperature ceramic superconductors

DOEpatents

Wu, Weite; Chu, Cha Y.; Goretta, Kenneth C.; Routbort, Jules L.

1995-01-01

A method and article of manufacture of a lead oxide based glass coating on a high temperature superconductor. The method includes preparing a dispersion of glass powders in a solution, applying the dispersion to the superconductor, drying the dispersion before applying another coating and heating the glass powder dispersion at temperatures below oxygen diffusion onset and above the glass melting point to form a continuous glass coating on the superconductor to establish compressive stresses which enhance the fracture strength of the superconductor.

Attaching Copper Wires to Magnetic-Reed-Switch Leads

NASA Technical Reports Server (NTRS)

Kamila, Rudolf

1987-01-01

Bonding method reliably joins copper wires to short iron-alloy leads from glass-encased dry magnetic-reed switch without disturbing integrity of glass-to-metal seal. Joint resistant to high temperatures and has low electrical resistance.

Method of making an integral window hermetic fiber optic component

DOEpatents

Dalton, R.D.; Kramer, D.P.; Massey, R.T.; Waker, D.A.

1996-11-12

In the fabrication of igniters, actuators, detonators, and other pyrotechnic devices to be activated by a laser beam, an integral optical glass window is formed by placing a preform in the structural member of the device and then melting the glass and sealing it in place by heating at a temperature between the ceramming temperature of the glass and the melting point of the metal, followed by rapid furnace cooling to avoid devitrification. No other sealing material is needed to achieve hermeticity. A preferred embodiment of this type of device is fabricated by allowing the molten glass to flow further and form a plano-convex lens integral with and at the bottom of the window. The lens functions to decrease the beam divergence caused by refraction of the laser light passing through the window when the device is fired by means of a laser beam. 9 figs.

Method of making an integral window hermetic fiber optic component

DOEpatents

Dalton, Rick D.; Kramer, Daniel P.; Massey, Richard T.; Waker, Damon A.

1996-11-12

In the fabrication of igniters, actuators, detonators, and other pyrotechnic devices to be activated by a laser beam, an integral optical glass window is formed by placing a preform in the structural member of the device and then melting the glass and sealing it in place by heating at a temperature between the ceramming temperature of the glass and the melting point of the metal, followed by rapid furnace cooling to avoid devitrification. No other sealing material is needed to achieve hermeticity. A preferred embodiment of this type of device is fabricated by allowing the molten glass to flow further and form a plano-convex lens integral with and at the bottom of the window. The lens functions to decrease the beam divergence caused by refraction of the laser light passing through the window when the device is fired by means of a laser beam.

Low-temperature hermetic sealing of optical fiber components

DOEpatents

Kramer, D.P.

1996-10-22

A method for manufacturing low-temperature hermetically sealed optical fiber components is provided. The method comprises the steps of: inserting an optical fiber into a housing, the optical fiber having a glass core, a glass cladding and a protective buffer layer disposed around the core and cladding; heating the housing to a predetermined temperature, the predetermined temperature being below a melting point for the protective buffer layer and above a melting point of a solder; placing the solder in communication with the heated housing to allow the solder to form an eutectic and thereby fill a gap between the interior of the housing and the optical fiber; and cooling the housing to allow the solder to form a hermetic compression seal between the housing and the optical fiber. 5 figs.

Low-temperature hermetic sealing of optical fiber components

DOEpatents

Kramer, Daniel P.

1996-10-22

A method for manufacturing low-temperature hermetically sealed optical fi components is provided. The method comprises the steps of: inserting an optical fiber into a housing, the optical fiber having a glass core, a glass cladding and a protective buffer layer disposed around the core and cladding; heating the housing to a predetermined temperature, the predetermined temperature being below a melting point for the protective buffer layer and above a melting point of a solder; placing the solder in communication with the heated housing to allow the solder to form an eutectic and thereby fill a gap between the interior of the housing and the optical fiber; and cooling the housing to allow the solder to form a hermetic compression seal between the housing and the optical fiber.

Hermetic diode laser transmitter module

NASA Astrophysics Data System (ADS)

Ollila, Jyrki; Kautio, Kari; Vahakangas, Jouko; Hannula, Tapio; Kopola, Harri K.; Oikarinen, Jorma; Sivonen, Matti

1999-04-01

In very demanding optoelectronic sensor applications it is necessary to encapsulate semiconductor components hermetically in metal housings to ensure reliable operation of the sensor. In this paper we report on the development work to package a laser diode transmitter module for a time- off-light distance sensor application. The module consists of a lens, laser diode, electronic circuit and optomechanics. Specifications include high acceleration, -40....+75 degree(s)C temperature range, very low gas leakage and mass-production capability. We have applied solder glasses for sealing optical lenses and electrical leads hermetically into a metal case. The lens-metal case sealing has been made by using a special soldering glass preform preserving the optical quality of the lens. The metal housings are finally sealed in an inert atmosphere by welding. The assembly concept to retain excellent optical power and tight optical axis alignment specifications is described. The reliability of the laser modules manufactured has been extensively tested using different aging and environmental test procedures. Sealed packages achieve MIL- 883 standard requirements for gas leakage.

Reliability evaluation of hermetic dual in-line flat microcircuit packages

NASA Technical Reports Server (NTRS)

Johnson, G. M.; Conaway, L. K.

1977-01-01

The relative strengths and weaknesses of 35 commonly used hermetic flat and dual in-line packages were determined and used to rank each of the packages according to a numerical weighting scheme for package attributes. The list of attributes included desirable features in five major areas: lead and lead seal, body construction, body materials, lid and lid seal, and marking. The metal flat pack and multilayer integral ceramic flat pack and DIP received the highest rankings, and the soft glass Cerdip and Cerpak types received the lowest rankings. Loss of package hermeticity due to lead and lid seal problems was found to be the predominant failure mode from the literature/data search. However, environmental test results showed that lead and lid seal failures due to thermal stressing was only a problem with the hard glass (Ceramic) body DIP utilizing a metal lid and/or bottom. Insufficient failure data were generated for the other package types tested to correlate test results with the package ranking.

Facilitated giga-seal formation with a just originated glass surface.

PubMed

Böhle, T; Benndorf, K

1994-07-01

A simple technique of tip preparation in patch pipettes is described, which facilitates giga-seal formation. The pipettes were fabricated from thick-walled borosilicate glass tubing (external diameter 2.0 mm, internal diameter 0.5 mm) and the tips could be repeatedly broken in the bath. The pipette resistance correspondingly fell in steps of 3-20 M omega from about 80 M omega to about 2 M omega (double concentrated Tyrode). Scanning electron microscopy showed that the tip obtained after breaking was fairly plain. These broken tips were especially appropriate for patch-clamping. In cardiac myocytes in 11 out of 26 patches with Na+ channel activity, giga-seals developed spontaneously, i.e. without suction. In these patches the amplitude of the mean current with depolarizing pulses to -40 mV was significantly higher in comparison with patches formed under negative pressure. It is concluded that spontaneously sealed patches are most likely of planar configuration and the Na+ channel activity exceeds that in suction-induced patches.

Development of a Mechanistic-Based Healing Model for Self-Healing Glass Seals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Wei; Stephens, Elizabeth V.; Sun, Xin

Self-healing glass, a recent development of hermetic sealant materials, has the ability to effectively repair damage when heated to elevated temperatures; thus, able to extend its service life. Since crack healing morphological changes in the glass material are usually temperature and stress dependent, quantitative studies to determine the effects of thermo-mechanical conditions on the healing behavior of the self-healing glass sealants are extremely useful to accommodate the design and optimization of the sealing systems within SOFCs. The goal of this task is to develop a mechanistic-based healing model to quantify the stress and temperature dependent healing behavior. A two-step healingmore » mechanism was developed and implemented into finite element (FE) models through user-subroutines. Integrated experimental/kinetic Monte Carlo (kMC) simulation methodology was taken to calibrate the model parameters. The crack healing model is able to investigate the effects of various thermo-mechanical factors; therefore, able to determine the critical conditions under which the healing mechanism will be activated. Furthermore, the predicted results can be used to formulate the continuum damage-healing model and to assist the SOFC stack level simulations in predicting and evaluating the effectiveness and the performance of various engineering seal designs.« less

Characterization of Fast-Scan Cyclic Voltammetric Electrodes Using Paraffin as an Effective Sealant with In Vitro and In Vivo Applications.

PubMed

Ramsson, Eric S; Cholger, Daniel; Dionise, Albert; Poirier, Nicholas; Andrus, Avery; Curtiss, Randi

2015-01-01

Fast-scan cyclic voltammetry (FSCV) is a powerful technique for measuring sub-second changes in neurotransmitter levels. A great time-limiting factor in the use of FSCV is the production of high-quality recording electrodes; common recording electrodes consist of cylindrical carbon fiber encased in borosilicate glass. When the borosilicate is heated and pulled, the molten glass ideally forms a tight seal around the carbon fiber cylinder. It is often difficult, however, to guarantee a perfect seal between the glass and carbon. Indeed, much of the time spent creating electrodes is in an effort to find a good seal. Even though epoxy resins can be useful in this regard, they are irreversible (seals are permanent), wasteful (epoxy cannot be reused once hardener is added), hazardous (hardeners are often caustic), and require curing. Herein we characterize paraffin as an electrode sealant for FSCV microelectrodes. Paraffin boasts the advantages of near-immediate curing times, simplicity in use, long shelf-life and stable waterproof seals capable of withstanding extended cycling. Borosilicate electrode tips were left intact or broken and dipped in paraffin embedding wax. Excess wax was removed from the carbon surface with xyelenes or by repeated cycling at an extended waveform (-0.4 to 1.4V, 400 V/s, 60 Hz). Then, the waveform was switched to a standard waveform (-0.4 to 1.3V, 400 V/s, 10 Hz) and cycled until stable. Wax-sealing does not inhibit electrode sensitivity, as electrodes detected linear changes in dopamine before and after wax (then xylenes) exposure. Paraffin seals are intact after 11 days of implantation in the mouse, and still capable of measuring transient changes in in vivo dopamine. From this it is clear that paraffin wax is an effective sealant for FSCV electrodes that provides a convenient substitute to epoxy sealants.

Characterization of Fast-Scan Cyclic Voltammetric Electrodes Using Paraffin as an Effective Sealant with In Vitro and In Vivo Applications

PubMed Central

Ramsson, Eric S.; Cholger, Daniel; Dionise, Albert; Poirier, Nicholas; Andrus, Avery; Curtiss, Randi

2015-01-01

Fast-scan cyclic voltammetry (FSCV) is a powerful technique for measuring sub-second changes in neurotransmitter levels. A great time-limiting factor in the use of FSCV is the production of high-quality recording electrodes; common recording electrodes consist of cylindrical carbon fiber encased in borosilicate glass. When the borosilicate is heated and pulled, the molten glass ideally forms a tight seal around the carbon fiber cylinder. It is often difficult, however, to guarantee a perfect seal between the glass and carbon. Indeed, much of the time spent creating electrodes is in an effort to find a good seal. Even though epoxy resins can be useful in this regard, they are irreversible (seals are permanent), wasteful (epoxy cannot be reused once hardener is added), hazardous (hardeners are often caustic), and require curing. Herein we characterize paraffin as an electrode sealant for FSCV microelectrodes. Paraffin boasts the advantages of near-immediate curing times, simplicity in use, long shelf-life and stable waterproof seals capable of withstanding extended cycling. Borosilicate electrode tips were left intact or broken and dipped in paraffin embedding wax. Excess wax was removed from the carbon surface with xyelenes or by repeated cycling at an extended waveform (-0.4 to 1.4V, 400 V/s, 60 Hz). Then, the waveform was switched to a standard waveform (-0.4 to 1.3V, 400 V/s, 10 Hz) and cycled until stable. Wax-sealing does not inhibit electrode sensitivity, as electrodes detected linear changes in dopamine before and after wax (then xylenes) exposure. Paraffin seals are intact after 11 days of implantation in the mouse, and still capable of measuring transient changes in in vivo dopamine. From this it is clear that paraffin wax is an effective sealant for FSCV electrodes that provides a convenient substitute to epoxy sealants. PMID:26505195

Gas impermeable glaze for sealing a porous ceramic surface

DOEpatents

Reed, Scott T.; Stone, Ronald G.; Nenoff, Tina M.; Trudell, Daniel E.; Thoma, Steven G.

2004-04-06

A process for fabricating a gas impermeable seal on a porous ceramic surface using a thin, glass-based, pinhole free glaze. The process can be used to fabricate gas impermeable end seals on porous alumina tubes used as filter media. The porous alumina tubes can have an inorganic microporous thin film separation membrane on the inner surface, which can be used for high temperature gas separation processes.

Preparation of wafer-level glass cavities by a low-cost chemical foaming process (CFP).

PubMed

Shang, Jintang; Chen, Boyin; Lin, Wei; Wong, Ching-Ping; Zhang, Di; Xu, Chao; Liu, Junwen; Huang, Qing-An

2011-04-21

A novel foaming process-chemical foaming process (CFP)-using foaming agents to fabricate wafer-level micro glass cavities including channels and bubbles was investigated. The process consists of the following steps sequentially: (1) shallow cavities were fabricated by a wet etching on a silicon wafer; (2) powders of a proper foaming agent were placed in a silicon cavity, named 'mother cavity', on the etched silicon surface; (3) the silicon cavities were sealed with a glass wafer by anodic bonding; (4) the bonded wafers were heated to above the softening point of the glass, and baked for several minutes, when the gas released by the decomposition of the foaming agent in the 'mother cavity' went into the other sealed interconnected silicon cavities to foam the softened glass into cylindrical channels named 'daughter channels', or spherical bubbles named 'son bubbles'. Results showed that wafer-level micro glass cavities with smooth wall surfaces were achieved successfully without contamination by the CFP. A model for the CFP was proposed to predict the final shape of the glass cavity. Experimental results corresponded with model predictions. The CFP provides a low-cost avenue to preparation of micro glass cavities of high quality for applications such as micro-reactors, micro total analysis systems (μTAS), analytical and bio-analytical applications, and MEMS packaging.

Numerical analysis of melt-solid interface shapes and growth rates of gallium antimonide in a single-zone vertical Bridgman furnace

NASA Astrophysics Data System (ADS)

Dutta, P. S.; Bhat, H. L.; Kumar, Vikram

1995-09-01

Numerical analysis has been carried out to determine the deviation of the growth rate from the ampoule lowering rate and the shape of the isotherms during the growth of gallium antimonide using the vertical Bridgman technique in a single-zone furnace. Electrical analogues have been used to model the thermal behaviour of the growth system. The standard circuit analysis technique has been used to calculate the temperature distribution in the growing crystal under various growth conditions. The effects of furnace temperature gradient near the melt-solid interface, the ampoule lowering rate, the ampoule geometry, the thermal conductivity of the melt, the mode of heat extraction from the tip of the ampoule and the extent of lateral heat loss from the side walls of the ampoule on the shape of isotherms in the crystal have been evaluated. The theoretical results presented here agree well with our previously obtained experimental results.

Development of an Ultra-Pure, Carrier-Free 209Po Solution Standard

PubMed Central

Collé, R.; Fitzgerald, R. P.; Laureano-Perez, L.

2015-01-01

Ultra-pure, carrier-free 209Po solution standards have been prepared and standardized for their massic alpha-particle emission rate. The standards, which will be disseminated by the National Institute of Standards and Technology (NIST) as Standard Reference Material SRM 4326a, have a mean mass of (5.169 ± 0.003) g of a solution of polonium in nominal 2.0 mol▪L−1 HCl (having a solution density of (1.032 ± 0.002) g▪ mL−1 at 20 °C) that are contained in 5 mL, flame-sealed, borosilicate glass ampoules. They are certified to contain a 209Po massic alpha-particle emission rate of (39.01 ± 0.18) s−1▪g−1 as of a reference time of 1200 EST, 01 December 2013. This new standard series replaces SRM 4326 that was issued by NIST in 1994. The standardization was based on 4πα liquid scintillation (LS) spectrometry with two different LS counting systems and under wide variations in measurement and counting source conditions. The methodology for the standardization, with corrections for detection of the low-energy conversion electrons from the delayed 2 keV isomeric state in 205Pb and for the radiations accompanying the small 0.45 % electron-capture branch to 209Bi, involves a unique spectral analysis procedure that is specific for the case of 209Po decay. The entire measurement protocol is similar, but revised and improved from that used for SRM 4326. Spectroscopic impurity analyses revealed that no photon-emitting or alpha-emitting radionuclidic impurities were detected. The most common impurity associated with 209Po is 208Po and the activity ratio of 208Po/209Po was < 10−7. PMID:26958444

Luminescence of europium (III) complexes for visualization

NASA Astrophysics Data System (ADS)

Kolontaeva, Olga A.; Pozharov, Mikhail V.; Korolovich, Vladimir F.; Khokhlova, Anastasia R.; Kirdyanova, Anna N.; Burmistrova, Natalia A.; Zakharova, Tamara V.; Goryacheva, Irina Y.

2016-04-01

With the purpose to develop bright non-toxic luminescent label for theranostic application we have studied complexation of lanthanide dipicolinates (2,6-pyridinedicarboxylates) by sodium alginate and effect of thermal exposure of synthesized micro-capsules on their luminescent properties. Synthesized micro-capsules are stable in acidic medium but dissolve at pH ~ 4 due to transformation of cationic europium dipicolinate complex to anionic. Luminescence studies have shown that emission spectra of europium(III)-alginate complexes (both chloride and dipicolinate) contain two intensive bands characteristic to Eu3+ ion (5D0 --> 7F1 (590 nm) and 5D0 --> 7F1 (612 nm)). We have also found that at 160ºC europium(III)- alginate micro-capsules decompose to black, soot-like substance, therefore, their thermal treatment must be performed in closed environment (i.e., sealed ampoules).

Recent trends and future of pharmaceutical packaging technology

PubMed Central

Zadbuke, Nityanand; Shahi, Sadhana; Gulecha, Bhushan; Padalkar, Abhay; Thube, Mahesh

2013-01-01

The pharmaceutical packaging market is constantly advancing and has experienced annual growth of at least five percent per annum in the past few years. The market is now reckoned to be worth over $20 billion a year. As with most other packaged goods, pharmaceuticals need reliable and speedy packaging solutions that deliver a combination of product protection, quality, tamper evidence, patient comfort and security needs. Constant innovations in the pharmaceuticals themselves such as, blow fill seal (BFS) vials, anti-counterfeit measures, plasma impulse chemical vapor deposition (PICVD) coating technology, snap off ampoules, unit dose vials, two-in-one prefilled vial design, prefilled syringes and child-resistant packs have a direct impact on the packaging. The review details several of the recent pharmaceutical packaging trends that are impacting packaging industry, and offers some predictions for the future. PMID:23833515

Residual Gases in Crystal Growth Systems

NASA Technical Reports Server (NTRS)

Palosz, W.

2003-01-01

Residual gases present in closed ampoules may affect different crystal growth processes. That seems to be particularly true under microgravity conditions where, due to weightlessness of the melt, the gases may lead to detached solidification and/or formation of voids and bubbles, as observed in the past. For that reason a good understanding and control of formation of residual gases is important for an optimum design and meaningful interpretation of crystal growth experiments. Our extensive experimental and theoretical studies of the subject, summarized in this paper, include degassing of silica glass and generation of gases from different source materials. Different materials processing conditions, like outgassing under vacuum, annealing in hydrogen, resublimation, different material preparation procedures, multiple annealings, different processing times, and others were applied and their effect on the amount and composition of gas were analyzed. The experimental results were interpreted based on theoretical calculations on diffusion in silica glass and source materials and thermochemistry of the system. Procedures for a reduction of the amount of gas are also discussed.

Recent advances in Li/SO2 battery technology

NASA Astrophysics Data System (ADS)

Ralston, R. E.

The areas of improvement discussed are related to cell closure-hermetic seals, improved glass-to-metal seals, and lithium-limited cell design. Attention is given to the design of a Li/SO2 cell which can safely withstand discharge below zero volts into voltage reversal. The design characteristics of an unbalanced cell, the new lithium-limited or balanced cell, and a high rate unbalanced design are compared in a table for the 'D' size cell. It is concluded that the improvements in cell closure, glass seal stability, and cell balance have resulted in storability, reliability, and abuse resistance characteristics which make the performance of today's Li/SO2 battery without equal among competitive primary batteries. However, the Li/SO2 cell must not be used in applications where extreme electrical or environmental conditions can push the system beyond its recommended limits.

Two-Step Vapor/Liquid/Solid Purification

NASA Technical Reports Server (NTRS)

Holland, L. R.

1986-01-01

Vertical distillation system combines in single operation advantages of multiple zone refining with those of distillation. Developed specifically to load Bridgman-Stockbarger (vertical-solidification) growth ampoules with ultrapure tellurium and cadmium, system, with suitable modifications, serves as material refiner. In first phase of purification process, ampoule heated to drive off absorbed volatiles. Second phase, evaporator heated to drive off volatiles in charge. Third phase, slowly descending heater causes distillation from evaporator to growing crystal in ampoule.

Chamber for Growing and Observing Fungi

NASA Technical Reports Server (NTRS)

Pierson, Duane L.; Molina, Thomas C.

2005-01-01

A chamber has been designed to enable growth and observation of microcolonies of fungi in isolation from the external environment. Unlike prior fungus-growing apparatuses, this chamber makes it possible to examine a fungus culture without disrupting it. Partly resembling a small picture frame, the chamber includes a metal plate having a rectangular through-thethickness opening with recesses for a top and a bottom cover glass, an inlet for air, and an inlet for water. The bottom cover glass is put in place and held there by clips, then a block of nutrient medium and a moisture pad are placed in the opening. The block is inoculated, then the top cover glass is put in place and held there by clips. Once growth is evident, the chamber can be sealed with tape. Little (if any) water evaporates past the edges of the cover glasses, and, hence there is little (if any) need to add water. A microscope can be used to observe the culture through either cover glass. Because the culture is sealed in the chamber, it is safe to examine the culture without risking contamination. The chamber can be sterilized and reused.

Glass-ceramic hermetic seals to high thermal expansion metals

DOEpatents

Kramer, D.P.; Massey, R.T.

1987-04-28

A process for forming glass-ceramic materials from an alkaline silica-lithia glass composition comprising 60-72 mole-% SiO/sub 2/, 18-27 mole-% Li/sub 2/O, 0-5 mole-% Al/sub 2/O/sub 3/, 0-6 mole-% K/sub 2/O, 0-3 mole-% B/sub 2/O/sub 3/, and 0.5-2.5 mole-% P/sub 2/O/sub 5/, which comprises heating said glass composition at a first temperature within the 950-1050/degree/C range for 5-60 minutes, and then at a devitrification temperature within the 700-900/degree/C range for about 5-300 minutes to obtain a glass-ceramic having a thermal expansion coefficient of up to 210 x 10/sup /minus/7///degree/C. These ceramics form strong, hermetic seals with high expansion metals such as stainless steel alloys. An intermediate nucleation heating step conducted at a temperature within the range of 675-750/degree/C for 10-120 minutes may be employed between the first stage and the devitrification stage. 1 fig., 2 tabs.

High Reliability R-10 Windows Using Vacuum Insulating Glass Units

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stark, David

2012-08-16

The objective of this effort was for EverSealed Windows (“EverSealed” or “ESW”) to design, assemble, thermally and environmentally test and demonstrate a Vacuum Insulating Glass Unit (“VIGU” or “VIG”) that would enable a whole window to meet or exceed the an R-10 insulating value (U-factor ≤ 0.1). To produce a VIGU that could withstand any North American environment, ESW believed it needed to design, produce and use a flexible edge seal system. This is because a rigid edge seal, used by all other know VIG producers and developers, limits the size and/or thermal environment of the VIG to where themore » unit is not practical for typical IG sizes and cannot withstand severe outdoor environments. The rigid-sealed VIG’s use would be limited to mild climates where it would not have a reasonable economic payback when compared to traditional double-pane or triple-pane IGs. ESW’s goals, in addition to achieving a sufficiently high R-value to enable a whole window to achieve R-10, included creating a VIG design that could be produced for a cost equal to or lower than a traditional triple-pane IG (low-e, argon filled). ESW achieved these goals. EverSealed produced, tested and demonstrated a flexible edge-seal VIG that had an R-13 insulating value and the edge-seal system durability to operate reliably for at least 40 years in the harshest climates of North America.« less

INTEGRITY OF VOA-VIAL SEALS

EPA Science Inventory

Preservation of soil samples for the analysis of volatile organic compounds (VOCs) requires both the inhibition of VOC degradation and the restriction of vapor movement in or out of the sample container. Clear, 40,mL glass VOA vials manufactured by the four major U.S. glass manu...

Novel Bonding Technology for Hermetically Sealed Silicon Micropackage

NASA Astrophysics Data System (ADS)

Lee, Duck-Jung; Ju, Byeong-Kwon; Choi, Woo-Beom; Jeong, Jee-Won; Lee, Yun-Hi; Jang, Jin; Lee, Kwang-Bae; Oh, Myung-Hwan

1999-01-01

We performed glass-to-silicon bonding and fabricated a hermetically sealed silicon wafer using silicon direct bonding followed by anodic bonding (SDAB). The hydrophilized glass and silicon wafers in solution were dried and initially bonded in atmosphere as in the silicon direct bonding (SDB) process, but annealing at high temperature was not performed. Anodic bonding was subsequently carried out for the initially bonded specimens. Then the wafer pairs bonded by the SDAB method were different from those bonded by the anodic bonding process only. The effects of the bonding process on the bonded area and tensile strength were investigated as functions of bonding temperature and voltage. Using scanning electron microscopy (SEM), the cross-sectional view of the bonded interface region was observed. In order to investigate the migration of the sodium ions in the bonding process, the concentration of the bonded glass was compared with that of standard glass. The specimen bonded using the SDAB process had higher efficiency than that using the anodic bonding process only.

Rubber contact mechanics: adhesion, friction and leakage of seals.

PubMed

Tiwari, A; Dorogin, L; Tahir, M; Stöckelhuber, K W; Heinrich, G; Espallargas, N; Persson, B N J

2017-12-13

We study the adhesion, friction and leak rate of seals for four different elastomers: Acrylonitrile Butadiene Rubber (NBR), Ethylene Propylene Diene (EPDM), Polyepichlorohydrin (GECO) and Polydimethylsiloxane (PDMS). Adhesion between smooth clean glass balls and all the elastomers is studied both in the dry state and in water. In water, adhesion is observed for the NBR and PDMS elastomers, but not for the EPDM and GECO elastomers, which we attribute to the differences in surface energy and dewetting. The leakage of water is studied with rubber square-ring seals squeezed against sandblasted glass surfaces. Here we observe a strongly non-linear dependence of the leak rate on the water pressure ΔP for the elastomers exhibiting adhesion in water, while the leak rate depends nearly linearly on ΔP for the other elastomers. We attribute the non-linearity to some adhesion-related phenomena, such as dewetting or the (time-dependent) formation of gas bubbles, which blocks fluid flow channels. Finally, rubber friction is studied at low sliding speeds using smooth glass and sandblasted glass as substrates, both in the dry state and in water. The measured friction coefficients are compared to theory, and the origin of the frictional shear stress acting in the area of real contact is discussed. The NBR rubber, which exhibits the strongest adhesion both in the dry state and in water, also shows the highest friction both in the dry state and in water.

Assessing the Validity of the Simplified Potential Energy Clock Model for Modeling Glass-Ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jamison, Ryan Dale; Grillet, Anne M.; Stavig, Mark E.

Glass-ceramic seals may be the future of hermetic connectors at Sandia National Laboratories. They have been shown capable of surviving higher temperatures and pressures than amorphous glass seals. More advanced finite-element material models are required to enable model-based design and provide evidence that the hermetic connectors can meet design requirements. Glass-ceramics are composite materials with both crystalline and amorphous phases. The latter gives rise to (non-linearly) viscoelastic behavior. Given their complex microstructures, glass-ceramics may be thermorheologically complex, a behavior outside the scope of currently implemented constitutive models at Sandia. However, it was desired to assess if the Simplified Potential Energymore » Clock (SPEC) model is capable of capturing the material response. Available data for SL 16.8 glass-ceramic was used to calibrate the SPEC model. Model accuracy was assessed by comparing model predictions with shear moduli temperature dependence and high temperature 3-point bend creep data. It is shown that the model can predict the temperature dependence of the shear moduli and 3- point bend creep data. Analysis of the results is presented. Suggestions for future experiments and model development are presented. Though further calibration is likely necessary, SPEC has been shown capable of modeling glass-ceramic behavior in the glass transition region but requires further analysis below the transition region.« less

Study and Optimization on graft polymerization under normal pressure and air atmospheric conditions, and its application to metal adsorbent

NASA Astrophysics Data System (ADS)

Ueki, Yuji; Chandra Dafader, Nirmal; Hoshina, Hiroyuki; Seko, Noriaki; Tamada, Masao

2012-07-01

Radiation-induced graft polymerization of glycidyl methacrylate (GMA) onto non-woven polyethylene (NWPE) fabric was achieved under normal pressure and air atmospheric conditions, without using unique apparatus such as glass ampoules or vacuum lines. To attain graft polymerization under normal pressure and air atmospheric conditions, the effects of the pre-irradiation dose, pre-irradiation atmosphere, pre-irradiation temperature, de-aeration of GMA-emulsion, grafting atmosphere in a reactor, and dissolved oxygen (DO) concentration in GMA-emulsion on the degree of grafting (Dg) were investigated in detail. It was found that the DO concentration had the strongest influence, the pre-irradiation dose, de-aeration of emulsion and grafting atmosphere had a relatively strong impact, and the pre-irradiation atmosphere and pre-irradiation temperature had the least effect on Dg. The optimum DO concentration before grafting was 2.0 mg/L or less. When a polyethylene bottle was used as a reactor instead of a glass ampoule, graft polymerization under normal pressure and air atmospheric conditions could be achieved under the following conditions; the pre-irradiation dose was more than 50 kGy, the volume ratio of GMA-emulsion to air was 50:1 or less, and the DO concentration in GMA-emulsion during grafting was below 2.0 mg/L. Under these grafting conditions, Dg was controlled within a range of up to 362%. The prepared GMA-grafted NWPE (GMA-g-NWPE) fabric was modified with a phosphoric acid to obtain an adsorbent for heavy metal ions. In the column-mode adsorption tests of Pb(II), the adsorption performance of the produced phosphorylated GMA-g-NWPE fabric (fibrous metal adsorbent) was not essentially dependent on the flow rate of the feed. The breakthrough points of 200, 500, and 1000 h-1 in space velocity were 483, 477 and 462 bed volumes, and the breakthrough capacities of the three flow rates were 1.16, 1.15 and 1.16 mmol-Pb(II)/g-adsorbent.

Predicting the potential moisture ingress characteristics of polyisobutylene based edge seals (Conference Presentation)

NASA Astrophysics Data System (ADS)

Kempe, Michael D.

2016-09-01

Photovoltaic devices are often sensitive to moisture and must be packaged in such a way as to limit moisture ingress for 25 years or more. Typically, this is accomplished through the use of impermeable front and backsheets (e.g., glass sheets or metal foils). However, this will still allow moisture ingress between the sheets from the edges. Attempts to hermetically seal with a glass frit or similarly welded bonds at the edge have had problems with costs and mechanical strength. Because of this, low diffusivity polyisobutylene materials filled with desiccant are typically used. Although it is well known that these materials will substantially delay moisture ingress, correlating that to outdoor exposure has been difficult. Here, we use moisture ingress measurements at different temperatures and relative humidities to find fit parameters for a moisture ingress model for an edge-seal material. Then, using meteorological data, a finite element model is used to predict the moisture ingress profiles for hypothetical modules deployed in different climates and mounting conditions, assuming no change in properties of the edge-seal as a function of aging.

High thermal expansion sealing glass for use in radio frequency applications

DOEpatents

Kilgo, Riley D.; Brow, Richard K.; Kovacic, Larry

1999-01-01

The present invention provides a glass composition for hermetically sealing to high thermal expansion materials such as aluminum alloys, stainless steels, and copper alloys, which includes between about 10 and about 25 mole percent Na.sub.2 O, between about 10 and about 25 mole percent K.sub.2 O, between about 4 and about 15 mole percent Al.sub.2 O.sub.3, between about 35 and about 50 mole percent P.sub.2 O.sub.5, B.sub.2 O.sub.3 in a concentration not exceeding 10 mole percent, and MXO in a concentration not exceeding 12 mole percent, wherein MXO is a metal oxide selected from the group consisting of PbO, BaO, CaO and MgO or a mixture thereof. This composition is suitable to hermetically seal to components for use in RF-interconnection applications.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1989-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into an adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1987-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into and adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Applied Sciences Department (R&D) Patents; a Compilation

DTIC Science & Technology

1978-12-28

References Cited the first ampoule so that the two ampoules can he bro- UNITED STATES PATENTS ken simultaneously, and, upon mixing of the chemilu...Che-V222/541 miluminescent material and the other ampoule con-.tains an activator material. The almpoules can be bro-(561 References Cited ken by...Eaminer.-Robe" F. Stshl Aimmweys- Edgar J. broere. Ii. H Loach . and Paul S. isat `PYROTECHNCIGNALING ID E 1cER IT4 COMtPiOm WA!Eft EACTII’tIGN11M 4

European Science Notes. Volume 41, Number 9.

DTIC Science & Technology

1987-09-01

that by Robert W. Vest. PVDF is unique. It consists of a polar crystalline phase in an amorphous phase above the glass transition temperature at...sufficiently great that this technol- by glass -ceramic (solder glass ) bonding ogy is being seriously evaluated, of the disc to an alumina ring (for rela- 2...factors (GF = AR/R/e) which lower cost fabrication. Instead of using range in value from 2 to 18 depending on a solder glass seal as shown in Figure 1

In Vivo Effect of Calcium Hydroxide and Resin-modified Glass Ionomer Cement on Carious Dentin in Young Permanent Molars: An Ultrastructural and Macroscopic Study.

PubMed

Opal, Shireen; Garg, Shalini; Sharma, Deepak; Dhindsa, Abhishek; Jatana, Isha

2017-01-15

The purpose of this study was to evaluate macroscopically and ultrastructurally the effect of calcium hydroxide cement (CH) and resin-modified glass ionomer cement (RMGIC) compared with gutta percha (control) as a lining material on carious dentin after partial caries removal and sealing. Twenty-seven permanent molars with deep carious lesions underwent partial caries removal with the application of CH, RMGIC, or gutta percha (control) and were then sealed for three months. After a partial caries removal and sealing period, the dentin was macroscopically assessed (for color, consistency, and humidity) and further analyzed by scanning electron microscope to assess the ultrastructural changes in dentin (lumen size, mineralization of tubules, occlusion of tubules by cements, and bacterial ingress). The effect of treatment in each group was statistically analyzed. Dentin darkening and hardening were observed after the sealing period in all groups. However, there was no difference in the color after treatment among the three groups. It was observed that RMGIC showed a significant reduction in the size of the lumen compared to CH and the control. Partial caries removal and sealing resulted in dentin hardening, darkening, and dentin remineralization, irrespective of the dentin protection used.

Investigating Low Temperature Properties of Rubber Seals - 13020

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jaunich, M.; Wolff, D.; Stark, W.

To achieve the required tightness levels of containers for low and intermediate level radioactive wastes rubbers are widely applied as main sealing materials. The save encapsulation of the radioactive container contents has to be guaranteed according to legislation and appropriate guidelines for long storage periods as well as down to temperatures of -40 deg. C during transportation. Therefore the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance. It is known that the material properties of rubbers are strongly influenced by temperature. At low temperatures this is caused by the rubber-glass transition (abbr. glassmore » transition). During continuous cooling the material changes from rubber-like entropy-elastic to stiff energy-elastic behaviour, that allows nearly no strain or retraction. Therefore, rubbers are normally used above their glass transition but the minimum working temperature limit is not defined precisely, what can cause problems during application. The temperature range where full functionality is possible is strongly dependent on the application conditions and the material. For this investigation mainly ethylene propylene diene (EPDM) and fluorocarbon rubbers (FKM) were selected as they are often used for radioactive waste containers. Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) are typically used for the determination of the temperature range of the glass transition process. The standardized compression set measurement according to ISO 815 is common for investigation of rubber sealing materials as the test simulates the seal behaviour after release. To reduce the test time of the standard tests a faster technique giving the same information was developed. Additionally, the breakdown temperature of the sealing function of complete O-ring seals is measured in a component test setup to compare it with the results of the other tests. The experimental setup is capable of measuring the leakage rate at low temperatures by the pressure rise method. A model was developed that allows calculating the minimum working temperature limit of a seal by combining the results of the applied methods. (authors)« less

Transparent multi-zone crystal growth furnace and method for controlling the same

NASA Technical Reports Server (NTRS)

Batur, Celal (Inventor); Bennett, Robert J. (Inventor); Duval, Walter (Inventor)

2000-01-01

A crystal growth system, comprising: a furnace; a plurality of heating elements coupled to said furnace, each said plurality of heating elements defining a heat zone, each said heating element set to a desired temperature value; a plurality of thermocouples associated with respective heat zones to detect a temperature value; a translation system for passing an ampoule containing crystal growth material through said furnace into said heat zones and providing a positional location of said ampoule and; a multi-variable self-tuning temperature controller connected to said plurality of heating elements, said plurality of thermocouples and said translation system, said controller monitoring each said zone temperature value and upon considering the thermal interaction of heating zones and the moving thermal inertia of the ampoule, adjusting voltage input to said heat zones to obtain optimal crystal growth within said ampoule.

Transparent multi-zone crystal growth furnace and method for controlling the same

NASA Technical Reports Server (NTRS)

Batur, Celal (Inventor); Duval, Walter (Inventor); Bennett, Robert J. (Inventor)

2001-01-01

A crystal growth system, comprising: a furnace; a plurality of heating elements coupled to said furnace, each said plurality of heating elements defining a heat zone, each said heating element set to a desired temperature value; a plurality of thermocouples associated with respective heat zones to detect a temperature value; a translation system for passing an ampoule containing crystal growth material through said furnace into said heat zones and providing a positional location of said ampoule and; a multi-variable self-tuning temperature controller connected to said plurality of heating elements, said plurality of thermocouples and said translation system, said controller monitoring each said zone temperature value and upon considering the thermal interaction of heating zones and the moving thermal inertia of the ampoule, adjusting voltage input to said heat zones to obtain optimal crystal growth within said ampoule.

Pressurized heat treatment of glass ceramic

DOEpatents

Kramer, D.P.

1984-04-19

A method of producing a glass-ceramic having a specified thermal expansion value is disclosed. The method includes the step of pressurizing the parent glass material to a predetermined pressure during heat treatment so that the glass-ceramic produced has a specified thermal expansion value. Preferably, the glass-ceramic material is isostatically pressed. A method for forming a strong glass-ceramic to metal seal is also disclosed in which the glass-ceramic is fabricated to have a thermal expansion value equal to that of the metal. The determination of the thermal expansion value of a parent glass material placed in a high-temperature environment is also used to determine the pressure in the environment.

Pressurized heat treatment of glass-ceramic to control thermal expansion

DOEpatents

Kramer, Daniel P.

1985-01-01

A method of producing a glass-ceramic having a specified thermal expansion value is disclosed. The method includes the step of pressurizing the parent glass material to a predetermined pressure during heat treatment so that the glass-ceramic produced has a specified thermal expansion value. Preferably, the glass-ceramic material is isostatically pressed. A method for forming a strong glass-ceramic to metal seal is also disclosed in which the glass-ceramic is fabricated to have a thermal expansion value equal to that of the metal. The determination of the thermal expansion value of a parent glass material placed in a high-temperature environment is also used to determine the pressure in the environment.

Composite seals for liquid hydrogen and nuclear radiation environments.

NASA Technical Reports Server (NTRS)

Van Auken, R. L.; Chase, V. A.

1971-01-01

Description of plastic composite seals for service in a liquid-hydrogen and nuclear-radiation environment. The radiation-resistant aromatic heterocyclic class of polymers, including polyimide, polybenzimidazole, and polyquinoxaline, were evaluated for this application. The seal developed is based on a design involving a resin-starved laminate consisting of alternating layers of woven glass fabric and polymer film. This design imparts a mechanical spring characteristic to the seal, resulting in essentially complete elastic recovery when unloaded, and eliminates cold flow. Encapsulating techniques employing the polyquinoxaline polymer were developed which rendered the seal impervious to liquid hydrogen. The seals were tested before and after gamma irradiation up to 10 to the 10th ergs/g. Load/deflection and leakage tests were performed over a temperature range from -423 through +500 F.

INTEGRITY OF VOA-VIAL SEALS | Science Inventory | US ...

EPA Pesticide Factsheets

Preservation of soil samples for the analysis of volatile organic compounds (VOCs) requires both the inhibition of VOC degradation and the restriction of vapor movement in or out of the sample container. Clear, 40,mL glass VOA vials manufactured by the four major U.S. glass manufacturers were tested for seal integrity. Visual inspection revealed a variety of imperfections ranging from small indentations, bumps, and scratches on vial threads or lips, through obvious defects, such as large indentations or grooves in the vial lips and chipped or broken glass. The aluminum plate vacuum test proved to be unreliable in identifying potentially leaky vials. The septa-seal vacuum test was conducted twice on the 80 selected vials.Mean VOC concentrations after 14 days storage generally were within +- 20% of the known concentration with a majority of the concentrations within +- 15% of their known values. There were no statistically significant differences in VOC concentrations between vials in the potentially leaky and control group for any of the manufacturers. Only 1 vial lost VOCs and that was due to a large chip in the vial's lip and neck. These findings indicate that the silicone septa are flexible enough to overcome most vial imperfections and form a complete seal against VOC loss. A careful inspection of the VOA vials prior to use to remove any vials with large and obvious imperfections should be sufficient to screen out vials that are subject to VOC losses.

Thermally stable electrolytes for rechargeable lithium batteries, phase 2

NASA Technical Reports Server (NTRS)

Dominey, L. A.; Goldman, J. L.; Koch, V. R.

1989-01-01

During the second year of research under NASA SBIR Contract NAS7-967, Covalent Associates and NASA contract monitors at the Jet Propulsion Laboratory agreed to perform an evaluation of the three best electrolytes developed during Phase 2. Due to the extensive period of time required to collect meaningful cycling data, we realized the study would extend well beyond the original formal end of the Phase 2 program (August 31, 1988). The substitution of this effort in lieu of an earlier proposed 20-cell final deliverable is formally documented in Modification No. 1 of Contract NAS7-967 as task 7. This Addendum contains the results of the cycling studies performed at Covalent Associates. In addition, sealed ampoules of each of these three electrolytes were delivered to the Jet Propulsion Laboratory Electrochemical Power Group. Their concurrent evaluation in a different test vehicle has also been recently concluded and their results are also summarized herein.

Crystal growth from the vapor phase experiment MA-085

NASA Technical Reports Server (NTRS)

Wiedemeir, H.; Sadeek, H.; Klaessig, F. C.; Norek, M.

1976-01-01

Three vapor transport experiments on multicomponent systems were performed during the Apollo Soyuz mission to determine the effects of microgravity forces on crystal morphology and mass transport rates. The mixed systems used germanium selenide, tellurium, germanium tetraiodide (transport agent), germanium monosulfide, germanium tetrachloride (transport agent), and argon (inert atmosphere). The materials were enclosed in evacuated sealed ampoules of fused silica and were transported in a temperature gradient of the multipurpose electric furnace onboard the Apollo Soyuz spacecraft. Preliminary evaluation of 2 systems shows improved quality of space grown crystals in terms of growth morphology and bulk perfection. This conclusion is based on a direct comparison of space grown and ground based crystals by means of X-ray diffraction, microscopic, and chemical etching techniques. The observation of greater mass transport rates than predicted for a microgravity environment by existing vapor transport models indicates the existence of nongravity caused transport effects in a reactive solid/gas phase system.

Low temperature Zn diffusion for GaSb solar cell structures fabrication

NASA Technical Reports Server (NTRS)

Sulima, Oleg V.; Faleev, Nikolai N.; Kazantsev, Andrej B.; Mintairov, Alexander M.; Namazov, Ali

1995-01-01

Low temperature Zn diffusion in GaSb, where the minimum temperature was 450 C, was studied. The pseudo-closed box (PCB) method was used for Zn diffusion into GaAs, AlGaAs, InP, InGaAs and InGaAsP. The PCB method avoids the inconvenience of sealed ampoules and proved to be simple and reproducible. The special design of the boat for Zn diffusion ensured the uniformality of Zn vapor pressure across the wafer surface, and thus the uniformity of the p-GaSb layer depth. The p-GaSb layers were studied using Raman scattering spectroscopy and the x-ray rocking curve method. As for the postdiffusion processing, an anodic oxidation was used for a precise thinning of the diffused GaSb layers. The results show the applicability of the PCB method for the large-scale production of the GaSb structures for solar cells.

Thermally stable electrolytes for rechargeable lithium batteries, phase 2

NASA Astrophysics Data System (ADS)

Dominey, L. A.; Goldman, J. L.; Koch, V. R.

1989-09-01

During the second year of research under NASA SBIR Contract NAS7-967, Covalent Associates and NASA contract monitors at the Jet Propulsion Laboratory agreed to perform an evaluation of the three best electrolytes developed during Phase 2. Due to the extensive period of time required to collect meaningful cycling data, we realized the study would extend well beyond the original formal end of the Phase 2 program (August 31, 1988). The substitution of this effort in lieu of an earlier proposed 20-cell final deliverable is formally documented in Modification No. 1 of Contract NAS7-967 as task 7. This Addendum contains the results of the cycling studies performed at Covalent Associates. In addition, sealed ampoules of each of these three electrolytes were delivered to the Jet Propulsion Laboratory Electrochemical Power Group. Their concurrent evaluation in a different test vehicle has also been recently concluded and their results are also summarized herein.

Self-sealing of thermal fatigue and mechanical damage in fiber-reinforced composite materials

NASA Astrophysics Data System (ADS)

Moll, Jericho L.

Fiber reinforced composite tanks provide a promising method of storage for liquid oxygen and hydrogen for aerospace applications. The inherent thermal fatigue of these vessels leads to the formation of microcracks, which allow gas phase leakage across the tank walls. In this dissertation, self-healing functionality is imparted to a structural composite to effectively seal microcracks induced by both mechanical and thermal loading cycles. Two different microencapsulated healing chemistries are investigated in woven glass fiber/epoxy and uni-weave carbon fiber/epoxy composites. Self-healing of mechanically induced damage was first studied in a room temperature cured plain weave E-glass/epoxy composite with encapsulated dicyclopentadiene (DCPD) monomer and wax protected Grubbs' catalyst healing components. A controlled amount of microcracking was introduced through cyclic indentation of opposing surfaces of the composite. The resulting damage zone was proportional to the indentation load. Healing was assessed through the use of a pressure cell apparatus to detect nitrogen flow through the thickness direction of the damaged composite. Successful healing resulted in a perfect seal, with no measurable gas flow. The effect of DCPD microcapsule size (51 microm and 18 microm) and concentration (0--12.2 wt%) on the self-sealing ability was investigated. Composite specimens with 6.5 wt% 51 microm capsules sealed 67% of the time, compared to 13% for the control panels without healing components. A thermally stable, dual microcapsule healing chemistry comprised of silanol terminated poly(dimethyl siloxane) plus a crosslinking agent and a tin catalyst was employed to allow higher composite processing temperatures. The microcapsules were incorporated into a satin weave E-glass fiber/epoxy composite processed at 120°C to yield a glass transition temperature of 127°C. Self-sealing ability after mechanical damage was assessed for different microcapsule sizees (25 microm and 42 microm) and concentrations (0--11 vol%). Incorporating 9 vol% 42 microm capsules or 11 vol% 25 microm capsules into the composite matrix leads to 100% of the samples sealing. The effect of microcapsule concentration on the short beam strength, storage modulus, and glass transition temperature of the composite specimens was also investigated. The thermally stable tin catalyzed poly(dimethyl siloxane) healing chemistry was then integrated into a [0/90]s uniweave carbon fiber/epoxy composite. Thermal cycling (-196°C to 35°C) of these specimens lead to the formation of microcracks, over time, formed a percolating crack network from one side of the composite to the other, resulting in a gas permeable specimen. Crack damage accumulation and sample permeability was monitored with number of cycles for both self-healing and traditional non-healing composites. Crack accumulation occurred at a similar rate for all sample types tested. A 63% increase in lifetime extension was achieved for the self-healing specimens over traditional non-healing composites.

Packaged microsphere-taper coupling system with a high Q factor.

PubMed

Dong, Yongchao; Wang, Keyi; Jin, Xueying

2015-01-10

A novel packaged microsphere-taper coupling system which consists of a glass tube and two glass plates is proposed and demonstrated in this paper. We analyze the impact of the microsphere distortion on the resonant spectrum and it is observed that a very high quality factor (Q) up to 1.08×10(8) can be achieved by optimizing the microsphere position and orientation relative to the fiber taper. The maintenance of Q and a stable spectrum are realized by placing the packaged structure in a sealed organic glass box. Furthermore, to verify the practicability of the sealed device, thermal sensing experiments are carried out, which indicates the excellent convenience of the device with a resolution of 1.12×10(-4)°C. The portability and robustness of the packaged structure make it strikingly attractive and illustrate its potential in practical microcavity sensors and lasers.

Method and apparatus for an insulating glazing unit and compliant seal for an insulating glazing unit

DOEpatents

Francis, IV, William H.; Freebury, Gregg E.; Beidleman, Neal J.; Hulse, Michael

2016-05-03

A Vacuum Insulating Glazing Unit (VIGU) comprises two or more glass lites (panes) spaced apart from one another and hermetically bonded to an edge seal assembly therebetween. The resulting cavity between the lites is evacuated to create at least one insulating vacuum cavity within which are disposed a plurality of stand-off members to maintain separation between the lites. The edge seal assembly is preferably compliant in the longitudinal (i.e., edgewise) direction to allow longitudinal relative motion between the two lites (e.g., from thermal expansion). The longitudinal compliance may be obtained by imprinting a three-dimensional pattern into the edge seal material. The edge seal assembly is preferably bonded to the lites with a first bond portion that is hermetic and a second bond portion that is load-resistant. Methods for producing VIGUs and/or compliant edge seal assemblies and VIGU and edge seal apparatus are disclosed.

Crystallization behaviors and seal application of basalt based glass-ceramics

NASA Astrophysics Data System (ADS)

Ateş, A.; Önen, U.; Ercenk, E.; Yılmaz, Ş.

2017-02-01

Basalt based glass-ceramics were prepared by conventional melt-quenching technique and subsequently converted to glass-ceramics by a controlled nucleation and crystallization process. Glass materials were obtained by melt at 1500°C and quenched in cold water. The powder materials were made by milling and spin coating. The powders were applied on the 430 stainless steel interconnector material, and heat treatment was carried out. The interface characteristics between the glass-ceramic layer and interconnector were investigated by using X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The results showed that the basalt base glass-ceramic sealant material exhibited promising properties to use for SOFC.

Heat transfer simulation in a vertical Bridgman CdTe growth configuration

NASA Astrophysics Data System (ADS)

Martinez-Tomas, C.; Muñoz, V.; Triboulet, R.

1999-02-01

Modelling and numerical simulation of crystal growth processes have been shown to be powerful tools in order to understand the physical effects of different parameters on the growth conditions. In this study a finite difference/control volume technique for the study of heat transfer has been employed. This model takes into account the whole system: furnace temperature profile, air gap between furnace walls and ampoule, ampoule geometry, crucible coating if any, solid and liquid CdTe thermal properties, conduction, convection and radiation of heat and phase change. We have used the commercial code FLUENT for the numerical resolution that can be running on a personal computer. Results show that the temperature field is very sensitive to the charge and ampoule peculiarities. As a consequence, significant differences between the velocity of the ampoule and that of the isotherm determining the solid/liquid interface have been found at the onset of the growth.

Electron Temperature Measurements in an Argon/Cesium Plasma Diode.

DTIC Science & Technology

1987-12-01

treatment , Q~xC (E) is modeled as a linear function. Upon viewing the cesium cross section data, one notes that Qmx is reached within only 1 eV of...metal sealIC where the electrode leads enter the cell. Due to the shape of this seal, portions of the glass are exposed to the air, despite the aluminum

A technique for measuring the heat transfer coefficient inside a Bridgman furnace

NASA Technical Reports Server (NTRS)

Rosch, W.; Jesser, W.; Debnam, W.; Fripp, A.; Woodell, G.; Pendergrass, T. K.

1993-01-01

Knowledge of the amount of heat that is conducted, advected and radiated between an ampoule and the furnace is important for understanding vertical Bridgman crystal growth. This heat transfer depends on the temperature, emissivities and geometries of both the furnace and ampoule, as well as the choice of ambient gas inside the furnace. This paper presents a method which directly measures this heat transfer without the need to know any physical properties of the furnace, the ampoule, or the gaseous environment. Data are given for one specific furnace in which this method was used.

Intraorifice sealing ability of different materials in endodontically treated teeth: An in vitro study.

PubMed

Parekh, Bandish; Irani, Rukshin S; Sathe, Sucheta; Hegde, Vivek

2014-05-01

Microbial contamination of the pulp space is one of the major factors associated with endodontic failure. Thus, in addition to a three dimentional apical filling a coronal seal for root canal fillings has been recommended. The present study was conducted to evaluate and compare the intra-orifice sealing ability of three experimental materials after obturation of the root canal system. Fourty single rooted mandibular premolars were decoronated, cleaned, shaped and obturated. Gutta-percha was removed to the depth of 3.5 mm from the orifice with a heated plugger. Ten specimens each were sealed with Light Cure Glass Ionomer Cement (LCGIC), Flowable Composite (Tetric N-Flow), and Light Cure Glass Ionomer Cement with Flowable Composite in Sandwich Technique along with a positive control respectively and roots submerged in Rhodamine-B dye in vacuum for one week. Specimens were longitudinally sectioned and leakage measured using a 10X stereomicroscope and graded for depth of leakage. According to the results of the present study LC GIC + Tetric N Flow demonstrated significantly better seal (P < 0.01) than LC GIC. However there was no statistically significant difference in leakage (P > 0.01) between Tetric N-Flow and LCGIC+Tetric N-Flow groups. In the current study LCGIC+Tetric N-Flow was found to be superior over other experimental materials as intra-orifice barriers.

Preparation of 99Tcm-MAG3: no confirmation that sodium chloride injections from plastic containers affect radiochemical purity.

PubMed

Millar, A M; O'Brien, L M

1998-05-01

Reports have suggested that when sodium chloride injections from a plastic ampoule are used during the preparation of 99Tcm-mercaptoacetyltriglycine (99Tcm-MAG3), the radiochemical purity of the final product might be reduced. A study was therefore undertaken to examine the effect of sodium chloride injections from five manufacturers on the radiochemical purity and stability of 99Tcm-MAG3. One sodium chloride injection was supplied in a glass vial, three in plastic ampoules and one in a plastic infusion bag. Three batches of sodium chloride injections from each manufacturer were tested. The radiopharmaceutical was prepared at a radioactive concentration of 1.1 GBq in 10 ml according to the instructions of the manufacturer of TechneScan MAG3. Analysis of radiochemical purity was performed by high-performance liquid chromatography immediately after preparation and 6 h later. Using 95% as the minimum acceptable radiochemical purity, all the products were satisfactory over the 6 h test period. No manufacturer's sodium chloride injection was found to have a statistically significant effect on the radiochemical purity. Based on the 15 batches of sodium chloride injection tested, this study cannot confirm that sodium chloride injections from a plastic container affect the radiochemical purity of 99Tcm-MAG3. However, in view of the known sensitivity of some 99Tcm radiopharmaceuticals to external influences, it is probably good practice to test radiochemical purity when new batches of ancillary materials, such as sodium chloride injections, are introduced.

Preliminary Engineering Study of Long-Lead Time Equipment Required for Large Lightweight Mirror Manufacture

DTIC Science & Technology

1981-06-01

numnber) Annealing Fusion Sealed Mirrors ULED Mirrors Boule Large Lightweight Mirror Core Low Expansion Glass Coremaker Mirror Blanks Forming Furnace...Experiments 34 4 10.6 Grinder Procurement 35 J 1 I GLOSSARY Alpha - Coef. of thermal expansion. Boule - The disc of glass formed in the furnace. Cell...turning over of large plates, cores or mirrors. Flowout - Method used to produce large diameter plates from small diameter boules. Glass - Used in the

SUBSA and PFMI Transparent Furnace Systems Currently in use in the International Space Station Microgravity Science Glovebox

NASA Technical Reports Server (NTRS)

Spivey, Reggie A.; Gilley, Scott; Ostrogorsky, Aleksander; Grugel, Richard; Smith, Guy; Luz, Paul

2003-01-01

The Solidification Using a Baffle in Sealed Ampoules (SUBSA) and Pore Formation and Mobility Investigation (PFMI) furnaces were developed for operation in the International Space Station (ISS) Microgravity Science Glovebox (MSG). Both furnaces were launched to the ISS on STS-111, June 4, 2002, and are currently in use on orbit. The SUBSA furnace provides a maximum temperature of 850 C and can accommodate a metal sample as large as 30 cm long and 12mm in diameter. SUBSA utilizes a gradient freeze process with a minimum cooldown rate of 0.5C per min, and a stability of +/- 0.15C. An 8 cm long transparent gradient zone coupled with a Cohu 3812 camera and quartz ampoule allows for observation and video recording of the solidification process. PFMI is a Bridgman type furnace that operates at a maximum temperature of 130C and can accommodate a sample 23cm long and 10mm in diameter. Two Cohu 3812 cameras mounted 90 deg apart move on a separate translation system which allows for viewing of the sample in the transparent hot zone and gradient zone independent of the furnace translation rate and direction. Translation rates for both the cameras and furnace can be specified from 0.5micrometers/sec to 100 micrometers/sec with a stability of +/-5%. The two furnaces share a Process Control Module (PCM) which controls the furnace hardware, a Data Acquisition Pad (DaqPad) which provides signal condition of thermal couple data, and two Cohu 3812 cameras. The hardware and software allow for real time monitoring and commanding of critical process control parameters. This paper will provide a detailed explanation of the SUBSA and PFMI systems along with performance data and some preliminary results from completed on-orbit processing runs.

Electrochemical cell with high conductivity glass electrolyte

DOEpatents

Nelson, P.A.; Bloom, I.D.; Roche, M.F.

1986-04-17

A secondary electrochemical cell with sodium-sulfur or other molten reactants is provided with an ionically conductive glass electrolyte. The cell is contained within an electrically conductive housing with a first portion at negative potential and a second portion insulated therefrom at positive electrode potential. The glass electrolyte is formed into a plurality of elongated tubes and placed lengthwise within the housing. The positive electrode material, for instance sulfur, is sealed into the glass electrolyte tubes and is provided with an elongated axial current collector. The glass electrolyte tubes are protected by shield tubes or sheets that also define narrow annuli for wicking of the molten negative electrode material.

Electrochemical cell with high conductivity glass electrolyte

DOEpatents

Nelson, P.A.; Bloom, I.D.; Roche, M.F.

1987-04-21

A secondary electrochemical cell with sodium-sulfur or other molten reactants is provided with a ionically conductive glass electrolyte. The cell is contained within an electrically conductive housing with a first portion at negative potential and a second portion insulated therefrom at positive electrode potential. The glass electrolyte is formed into a plurality of elongated tubes and placed lengthwise within the housing. The positive electrode material, for instance sulfur, is sealed into the glass electrolyte tubes and is provided with an elongated axial current collector. The glass electrolyte tubes are protected by shield tubes or sheets that also define narrow annuli for wicking of the molten negative electrode material. 6 figs.

Electrochemical cell with high conductivity glass electrolyte

DOEpatents

Nelson, Paul A.; Bloom, Ira D.; Roche, Michael F.

1987-01-01

A secondary electrochemical cell with sodium-sulfur or other molten reactants is provided with a ionically conductive glass electrolyte. The cell is contained within an electrically conductive housing with a first portion at negative potential and a second portion insulated therefrom at positive electrode potential. The glass electrolyte is formed into a plurality of elongated tubes and placed lengthwise within the housing. The positive electrode material, for instance sulfur, is sealed into the glass electrolyte tubes and is provided with an elongated axial current collector. The glass electrolyte tubes are protected by shield tubes or sheets that also define narrow annuli for wicking of the molten negative electrode material.

Alkali-lead-iron phosphate glass and associated method

DOEpatents

Boatner, Lynn A.; Sales, Brian C.; Franco, Sofia C. S.

1994-01-01

A glass composition and method of preparation utilizes a mixture consisting of phosphorus oxide within the range of about 40 to 49 molar percent, lead oxide within the range of about 10 to 25 molar percent, iron oxide within the range of about 10 to 17 molar percent and an alkali oxide within the range of about 23 to 30 molar percent. The glass resulting from the melting and subsequent solidifying of the mixture possesses a high degree of durability and a coefficient of thermal expansion as high as that of any of a number of metals. Such features render this glass highly desirable in glass-to-metal seal applications.

Method and apparatus for dispensing small quantities of mercury from evacuated and sealed glass capsules

DOEpatents

Grossman, Mark W.; George, William A.; Pai, Robert Y.

1985-01-01

A technique for opening an evacuated and sealed glass capsule containing a material that is to be dispensed which has a relatively high vapor pressure such as mercury. The capsule is typically disposed in a discharge tube envelope. The technique involves the use of a first light source imaged along the capsule and a second light source imaged across the capsule substantially transversely to the imaging of the first light source. Means are provided for constraining a segment of the capsule along its length with the constraining means being positioned to correspond with the imaging of the second light source. These light sources are preferably incandescent projection lamps. The constraining means is preferably a multiple looped wire support.

Test Method Variability in Slow Crack Growth Properties of Sealing Glasses

NASA Technical Reports Server (NTRS)

Salem, J. A.; Tandon, R.

2010-01-01

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.

Improved Crystal Quality By Detached Solidification in Microgravity

NASA Technical Reports Server (NTRS)

Regel, Liya L.; Wilcox, William R.; Wang, Yaz-Hen; Wang, Jian-Bin

2003-01-01

Many microgravity directional solidification experiments yielded ingots with portions that grew without contacting the ampoule wall, leading to greatly improved crystallographic perfection. Our long term goals have been: (1) To develop a complete understanding of all of the phenomena of detached solidification.; (2) To make it possible to achieve detached solidification reproducibly; (3) To increase crystallographic perfection through detached solidification. We have three major achievements to report here: (1) We obtained a new material balance solution for the Moving Meniscus Model of detached solidification. This solution greatly clarifies the physics as well as the roles of the parameters in the system; (2) We achieved detached solidification of InSb growing on earth in BN-coated ampoules; (3) We performed an extensive series of experiments on freezing water that showed how to form multiple gas bubbles or tubes on the ampoule wall. However, these did not propagate around the wall and lead to fully detached solidification unless the ampoule wall was extremely rough and non-wetted.

Numerical simulation of CdTe vertical Bridgman growth

NASA Astrophysics Data System (ADS)

Ouyang, Hong; Shyy, Wei

1997-04-01

Numerical simulation has been conducted for steady-state Bridgman growth of the CdTe crystal with two ampoule configurations, namely, flat base and semi-spherical base. The present model accounts for conduction, convection and radiation, as well as phase change dynamics. The enthalpy formulation for phase change has been incorporated into a pressure-based algorithm with multi-zone curvilinear grid systems. The entire system which consists of the furnace enclosure wall, the encapsulated gas and the ampoule, contains irregularly configured domains. To meet the competing needs of producing accurate solutions with reasonable computing resources, a two-level approach is employed. The present study reveals that although the two ampoule configurations are quite different, their influence on the melt-solid interface shape is modest, and the undesirable concave interface appears in both cases. Since the interface shape strongly depends on thermal conductivities between the melt and the crystal, as well as ampoule wall temperature, accurate prescriptions of materials transport properties and operating environment are crucial for successful numerical predictions.

Bridgman Growth of GeSi Alloys in a Static Magnetic Field

NASA Technical Reports Server (NTRS)

Volz, M. P.; Szofran, F. R.; Vujisic, L.; Motakef, S.

1998-01-01

Ge(0.95)Si(0.050 alloy crystals have been grown by the vertical Bridgman technique, both with and without an axial 5 Tesla magnetic field. The crystals were processed in a constant axial thermal gradient and the effects of graphite, hot pressed boron nitride, and pyrolitic boron nitride ampoule materials on interface shapes and macrosegregation profiles were investigated. The sample grown in a graphite ampoule at 5 Tesla exhibited a macroscopic axial concentration profile close to that of complete mixing and strong striation patterns. In samples grown in boron nitride ampoules, both with and without a 5 Tesla magnetic field applied, measured macroscopic axial concentration profiles were intermediate between those expected for a completely mixed melt and diffusion-controlled growth, and striation patterns were also observed. Possible explanations for the apparent inability of the magnetic field to reduce the flow velocities to below the growth velocities are discussed, and results of growth experiments in pyrolitic boron nitride ampoules are also described.

A numerical study of thermal conditions in the THM growth of HgTe

NASA Astrophysics Data System (ADS)

Martínez-Tomás, M. C.; Muñoz-Sanjosé, V.; Reig, C.

2002-09-01

A numerical simulation of the travelling heater method (THM) process in the growth of HgTe is carried out. The whole system (furnace, ampoule and charge) is taken into account in the frame of a quasi-steady-state model. The mass conservation condition for the solute in the liquid zone permits the determination of the rate of advance of the crystallisation isotherm as a function of the heater position. We claim to study the evolution of different magnitudes along the growth process, searching for the physical reasons which could be at the origin of defects in the form of thin layers observed in some growing experiences. To solve the governing equations of fluid flow, heat transfer and mass transport we have made use of a commercial code which can run in a PC. The simulation is made by using a three-level strategy, which allows the reduction of the computational effort. In the first level, heat transport is assumed to be by conduction, convection and radiation between the furnace and the ampoule, and by conduction through the ampoule wall, coating, solid and liquid zones. The temperature calculated at this level in the air/ampoule boundary is used as boundary condition for the second and third level. In these two levels the ampoule and its content are studied in detail. Convection in the liquid zone is considered at the second level and thermosolutal convection is finally included at the third level. The analysis of the incoming/outcoming heat flux per second through the ampoule for the whole system shows that the lower part of the ampoule exhibits some ineffectiveness for the heat evacuation at certain positions of the growth run, depending on thermal properties of the whole system and the particular material to be grown. As a consequence, the growth rate suffers a significant variation just for these positions of the heater. From these considerations a plausible interpretation has been proposed to understand the apparition of solvent inclusions in the form of thin layers when a material as HgTe is grown by the THM method.

Effect of convection on the microstructure of the MnBi/Bi eutectic

NASA Technical Reports Server (NTRS)

Eisa, Gaber Faheem; Wilcox, william R.; Busch, Garrett

1986-01-01

For the quasi-regular fibrous microstructure of MnBi formed at freezing rates of 9 mm/h and above, good agreement between experimental and theoretical results for fiber spacing, freezing rate, radial position, and ampoule rotation rate is found. For the irregular blade-like microstructure formed at lower freezing rates, convection is found to coarsen the microstructure somwhat more than predicted. The volume fraction of MnBi was also shown to depend on ampoule rotation and radial position, even in the absence of ampoule rotation. The two-fold finer microstructure observed in space-processed material could not be explained by the elimination of buoyancy-driven natural convection.

Handbook of Pressure-Proof Connector and Cable Harness Design for Sonar Systems.

DTIC Science & Technology

1981-12-21

as delrin, polycarbonate, epoxy, melamine , and diallyl phthalate were evaluated. Glass -filled diallyl phthalate was the only candidate material which...and at 900 intervals on the bulk- head of glass sealed receptacles, 0.125 inch from the outermost glass bead . 7-3 :1 7.2.1.5 The area of the component...in their ability to cure resins , as well as their tendency to cause skin irritation or dermatitis. Most room temperature-set hardeners are based on

Chemically durable nitrogen containing phosphate glasses useful for sealing to metals

DOEpatents

Day, Delbert E.; Wilder, Jr., James A.

1984-01-01

The chemical durability of alkali phosphate glasses is improved by incorporation of up to 23 weight percent of nitrogen. A typical phosphate glass contains: 10 to 60 mole % of Li.sub.2 O, Na.sub.2 O or K.sub.2 O; 5-40 mole % of BaO or CAO; 0-1 to 10 mole % of Al.sub.2 O.sub.3 ; and 40-70 mole % of P.sub.2 O.sub.5. Nitrides, such as AlN, are the favored additives.

Tamper-indicating device having a glass body

DOEpatents

Johnston, Roger G.; Garcia, Anthony R. E.

2003-04-29

A tamper-indicating device is described. The device has a first glass body member and a second glass body member that are attached to each other through a hasp. The glass body members of the device can be tempered. The body members can be configured with hollow volumes into which powders, microparticles, liquids, gels, or combinations thereof are sealed. The choice, the amount, and the location of these materials can produce a visible, band pattern to provide each body member with a unique fingerprint identifier, which makes it extremely difficult to repair or replace once it is damaged in order to avoid tamper detection.

Method of forming capsules containing a precise amount of material

DOEpatents

Grossman, Mark W.; George, William A.; Maya, Jakob

1986-01-01

A method of forming a sealed capsule containing a submilligram quantity of mercury or the like, the capsule being constructed from a hollow glass tube, by placing a globule or droplet of the mercury in the tube. The tube is then evacuated and sealed and is subsequently heated so as to vaporize the mercury and fill the tube therewith. The tube is then separated into separate sealed capsules by heating spaced locations along the tube with a coiled heating wire means to cause collapse spaced locations therealong and thus enable separation of the tube into said capsules.

Method of forming capsules containing a precise amount of material

DOEpatents

Grossman, M.W.; George, W.A.; Maya, J.

1986-06-24

A method of forming a sealed capsule containing a submilligram quantity of mercury or the like, the capsule being constructed from a hollow glass tube, by placing a globule or droplet of the mercury in the tube. The tube is then evacuated and sealed and is subsequently heated so as to vaporize the mercury and fill the tube therewith. The tube is then separated into separate sealed capsules by heating spaced locations along the tube with a coiled heating wire means to cause collapse spaced locations there along and thus enable separation of the tube into said capsules. 7 figs.

Engineered high expansion glass-ceramics having near linear thermal strain and methods thereof

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dai, Steve Xunhu; Rodriguez, Mark A.; Lyon, Nathanael L.

The present invention relates to glass-ceramic compositions, as well as methods for forming such composition. In particular, the compositions include various polymorphs of silica that provide beneficial thermal expansion characteristics (e.g., a near linear thermal strain). Also described are methods of forming such compositions, as well as connectors including hermetic seals containing such compositions.

Novel MEMS Apparatus for In Situ Thermo-Mechanical Tensile Testing of Materials at the Micro- and Nano-Scale (Preprint)

DTIC Science & Technology

2009-04-01

outer ends of the MEMS-stage connect the stage to a macroscopic piezo -electric actuated test frame using rigid pins. In order to apply uniaxial...carbide also served as the resistor for Joule heating. This heater was used to melt glass (Soda lime glass, softening temperature: 720C, Gold Seal

Air Sparging Design Paradigm

DTIC Science & Technology

2002-08-12

treatment zone increases with increasing separation. It is important to ensure a good annular air flow seal between the top of the screened interval and... seals are critical to successful air sparging operation. In their absence, the injected air will flow up along the well bore and the well will be...glass beads and model homogenous and heterogeneous subsurface hydrogeologic settings were simulated . The goal of the study was to observe how the

Chronic cranial window with access port for repeated cellular manipulations, drug application, and electrophysiology

PubMed Central

Roome, Christopher J.; Kuhn, Bernd

2014-01-01

Chronic cranial windows have been instrumental in advancing optical studies in vivo, permitting long-term, high-resolution imaging in various brain regions. However, once a window is attached it is difficult to regain access to the brain under the window for cellular manipulations. Here we describe a simple device that combines long term in vivo optical imaging with direct brain access via glass or quartz pipettes and metal, glass, or quartz electrodes for cellular manipulations like dye or drug injections and electrophysiological stimulations or recordings while keeping the craniotomy sterile. Our device comprises a regular cranial window glass coverslip with a drilled access hole later sealed with biocompatible silicone. This chronic cranial window with access port is cheap, easy to manufacture, can be mounted just as the regular chronic cranial window, and is self-sealing after retraction of the pipette or electrode. We demonstrate that multiple injections can be performed through the silicone port by repetitively bolus loading calcium sensitive dye into mouse barrel cortex and recording spontaneous cellular activity over a period of weeks. As an example to the extent of its utility for electrophysiological recording, we describe how simple removal of the silicone seal can permit patch pipette access for whole-cell patch clamp recordings in vivo. During these chronic experiments we do not observe any infections under the window or impairment of animal health. PMID:25426027

Flip the tip: an automated, high quality, cost-effective patch clamp screen.

PubMed

Lepple-Wienhues, Albrecht; Ferlinz, Klaus; Seeger, Achim; Schäfer, Arvid

2003-01-01

The race for creating an automated patch clamp has begun. Here, we present a novel technology to produce true gigaseals and whole cell preparations at a high rate. Suspended cells are flushed toward the tip of glass micropipettes. Seal, whole-cell break-in, and pipette/liquid handling are fully automated. Extremely stable seals and access resistance guarantee high recording quality. Data obtained from different cell types sealed inside pipettes show long-term stability, voltage clamp and seal quality, as well as block by compounds in the pM range. A flexible array of independent electrode positions minimizes consumables consumption at maximal throughput. Pulled micropipettes guarantee a proven gigaseal substrate with ultra clean and smooth surface at low cost.

Alkali-lead-iron phosphate glass and associated method

DOEpatents

Boatner, L.A.; Sales, B.C.; Franco, S.C.S.

1994-03-29

A glass composition and method of preparation utilizes a mixture consisting of phosphorus oxide within the range of about 40 to 49 molar percent, lead oxide within the range of about 10 to 25 molar percent, iron oxide within the range of about 10 to 17 molar percent and an alkali oxide within the range of about 23 to 30 molar percent. The glass resulting from the melting and subsequent solidifying of the mixture possesses a high degree of durability and a coefficient of thermal expansion as high as that of any of a number of metals. Such features render this glass highly desirable in glass-to-metal seal applications. 6 figures.

Convection of tin in a Bridgman system. II - An electrochemical method for detecting flow regimes

NASA Technical Reports Server (NTRS)

Sears, B.; Fripp, A. L.; Debnam, W. J., Jr.; Woodell, G. A.; Anderson, T. J.; Narayanan, R.

1992-01-01

An ampoule was designed in order to obtain local flow behavior of the flow fields for convection of tin in a vertical Bridgman configuration. Multiple electrochemical cells were located along the periphery of the ampoule. Oxygen was titrated into the ampoule at one of the cell locations using a potentiostat and the concentration of oxygen was monitored at the other cell locations by operating the cells in a galvanic mode. Onset of oscillations were detected by means of thermocouples. We conclude that the flows are generally three dimensional for an aspect ratio of 5. Results on oscillations concurred with those of earlier workers. Suggestions for improved designs were made.

Production of Reference Enteroviruses

PubMed Central

Kalter, S. S.; Rodriguez, A. R.; Armour, V.

1968-01-01

Forty-five human enterovirus reagents of certified purity and quality were prepared for use as seed viruses and as immunizing antigens. One of the reagents was ampouled as “untreated” seed virus, whereas 14 were ampouled as “MgCl2-stabilized” reagents. The remaining 30 reagents were ampouled as “untreated” seed viruses and as “MgCl2-stabilized” reagents. Thirty of the reagents were propagated on primary African green monkey kidney cells, 3 on primary baboon kidney cells, 3 on primary rhesus monkey kidney cells, and the remaining 9 on human amnion cells. Forty-two of the viral antigens were concentrated for use in the production of high-titered specific antisera in large animals. PMID:4300898

Isothermal Dendritic Growth Experiment - Science, engineering, and hardware development for USMP space flights

NASA Technical Reports Server (NTRS)

Glicksman, M. E.; Hahn, R. C.; Koss, M. B.; Tirmizi, S. H.; Selleck, M. E.; Velosa, A.; Winsa, E.

1991-01-01

The Isothermal Dendritic Growth Experiment (IDGE) has been designed to provide microgravity data on dendritic growth for a critical test of theory. This paper updates progress on constructing a crystal growth chamber suitable for space flight. The IDGE chamber is constructed from glass and stainless steel and is hermetically sealed by electron beam welds and glass-metal seals. Initial tests of the chambers sample's melting point plateau show that the new chamber design is capable of preserving the 99.9995 percent purity of succinonitrile. Dendrite growth can be initiated in the center of the IDGE chamber by means of thermo-electric coolers and a capillary injector tube (stinger). The new IDGE chamber is ready for fully integrated tests with the prototype IDGE engineering hardware at NASA's Lewis Research Center.

Method and apparatus for dispensing small quantities of mercury from evacuated and sealed glass capsules

DOEpatents

Grossman, M.W.; George, W.A.; Pai, R.Y.

1985-08-13

A technique is disclosed for opening an evacuated and sealed glass capsule containing a material that is to be dispensed which has a relatively high vapor pressure such as mercury. The capsule is typically disposed in a discharge tube envelope. The technique involves the use of a first light source imaged along the capsule and a second light source imaged across the capsule substantially transversely to the imaging of the first light source. Means are provided for constraining a segment of the capsule along its length with the constraining means being positioned to correspond with the imaging of the second light source. These light sources are preferably incandescent projection lamps. The constraining means is preferably a multiple looped wire support. 6 figs.

Influence of various bonding techniques on the fracture strength of thin CAD/CAM-fabricated occlusal glass-ceramic veneers.

PubMed

Yazigi, Christine; Kern, Matthias; Chaar, Mohamed Sad

2017-11-01

To evaluate the efficiency of immediate dentin sealing and the effects of different bonding protocols on the fracture strength of CAD/CAM occlusal veneers bonded to exposed dentin. Ninety-six extracted maxillary premolars were initially divided into three main groups with 32 specimens each: without immediate dentin sealing, immediate dentin sealing/total etching and immediate dentin sealing/selective etching. Teeth were identically prepared in the dentin to receive occlusal veneers of 0.8mm thickness, milled from lithium disilicate ceramic blocks (IPS e.max CAD). Each main group was later subdivided, according to the pre-cementation surface etching protocol (total/selective), into two subgroups with 16 specimens each. All restorations were adhesively bonded using a resin cement (Variolink Esthetic). Half of the specimens of each subgroup were subjected to thermo-dynamic loading in a chewing simulator with 1,200,000 cycles at 10kg load. The other half and the surviving specimens were subjected to quasi-static loading until failure. Statistical analysis was performed using three-way ANOVA and Tukey's post-hoc tests. All specimens except one survived the artificial aging. A significantly higher fracture strength of restorations (p ≤ 0.001) was obtained when immediate dentin sealing was followed regardless of the etching method with values ranging from a minimum of 1122 ± 336N to a maximum of 1853 ± 333N. Neither the pre-cementation treatment nor the artificial aging had a statistical significant effect on the fracture strength. Immediate dentin sealing protocol is recommended whenever dentin is exposed during the preparation for thin glass-ceramic occlusal veneers. Copyright © 2017 Elsevier Ltd. All rights reserved.

The Pharmaceutical Capping Process-Correlation between Residual Seal Force, Torque Moment, and Flip-off Removal Force.

PubMed

Mathaes, Roman; Mahler, Hanns-Christian; Vorgrimler, Lothar; Steinberg, Henrik; Dreher, Sascha; Roggo, Yves; Nieto, Alejandra; Brown, Helen; Roehl, Holger; Adler, Michael; Luemkemann, Joerg; Huwyler, Joerg; Lam, Philippe; Stauch, Oliver; Mohl, Silke; Streubel, Alexander

2016-01-01

The majority of parenteral drug products are manufactured in glass vials with an elastomeric rubber stopper and a crimp cap. The vial sealing process is a critical process step during fill-and-finish operations, as it defines the seal quality of the final product. Different critical capping process parameters can affect rubber stopper defects, rubber stopper compression, container closure integrity, and also crimp cap quality. A sufficiently high force to remove the flip-off button prior to usage is required to ensure quality of the drug product unit by the flip-off button during storage, transportation, and until opening and use. Therefore, the final product is 100% visually inspected for lose or defective crimp caps, which is subjective as well as time- and labor-intensive. In this study, we sealed several container closure system configurations with different capping equipment settings (with corresponding residual seal force values) to investigate the torque moment required to turn the crimp cap. A correlation between torque moment and residual seal force has been established. The torque moment was found to be influenced by several parameters, including diameter of the vial head, type of rubber stopper (serum or lyophilized) and type of crimp cap (West(®) or Datwyler(®)). In addition, we measured the force required to remove the flip-off button of a sealed container closure system. The capping process had no influence on measured forces; however, it was possible to detect partially crimped vials. In conclusion, a controlled capping process with a defined target residual seal force range leads to a tight crimp cap on a sealed container closure system and can ensure product quality. The majority of parenteral drug products are manufactured in a glass vials with an elastomeric rubber stopper and a crimp cap. The vial sealing process is a critical process step during fill-and-finish operations, as it defines the seal quality of the final product. An adequate force to remove the flip-off button prior to usage is required to ensure product quality during storage and transportation until use. In addition, the complete crimp cap needs to be fixed in a tight position on the vial. In this study, we investigated the torque moment required to turn the crimp cap and the force required to remove the flip-off button of container closure system sealed with different capping equipment process parameters (having different residual seal force values). © PDA, Inc. 2016.

Shock Reactivity of Non-Porous Mixtures of Manganese and Sulfur

NASA Astrophysics Data System (ADS)

Jette, Francois-Xavier; Goroshin, Samuel; Higgins, Andrew

2007-06-01

Stoichiometric mixtures of manganese powder and sulfur were melt-cast into solid pellets in order to study the mechanism of shock-enhanced reactivity in non-porous heterogeneous mixtures. This mixture was selected due to the large exothermic heat release of the manganese-sulfur reaction (214 kJ/mol), which causes the reaction to be self-sustaining once initiated. The test samples were placed in planar recovery ampoules and a strong shock was delivered via the detonation of a charge of amine-sensitized nitromethane. Various shock strengths were achieved by placing different thicknesses of PMMA attenuator between the explosive charge and the ampoule. The results confirmed that shock-induced reactions can be produced in the absence of porosity. Indeed, the critical shock pressure that caused ignition of the mixture in the ampoule was found to be in the range 2.2 - 3.8 GPa (pressures were estimated using LS-DYNA simulations). In the cases where the shock was too weak to cause ignition in the ampoule, the sample was extracted and its ignition temperature was determined using a differential thermal analyzer.

Chlorofluorocarbons, sulfur hexafluoride, and dissolved permanent gases in ground water from selected sites in and near the Idaho National Engineering and Environmental Laboratory, Idaho, 1994-97

USGS Publications Warehouse

Busenberg, Eurybiades; Plummer, Niel; Bartholomay, Roy C.; Wayland, Julian E.

1998-01-01

From July 1994 through May 1997, the U.S. Geological Survey in cooperation with the Department of Energy, sampled 86 wells completed in the Snake River Plain aquifer at and near the Idaho N ationa1 Engineering and Environmental Laboratory (INEEL). The wells were sampled for a variety of constituents including one- and two-carbon halocarbons. Concentrations of dichlorodifluoromethane (CFC-12), trichlorofluoromethane (CFC-11) and trichlorotrifluororoethane (CFC-113) were determined. The samples for halocarbon analysis were collected in 62-milliliter flame sealed borosilicate glass ampoules in the field. The data will be used to evaluate the ages of ground waters at INEEL. The ages of the ground water will be used to determine recharge rates, residence time, and travel time of water in the Snake River Plain aquifer in and near INEEL. The chromatograms of 139 ground waters are presented showing a large number of halomethanes, haloethanes, and haloethenes present in the ground waters underlying the INEEL. The chromatograms can be used to qualitatively evaluate a large number of contaminants at parts per trillion to parts per billion concentrations. The data can be used to study temporal and spatial distribution of contaminants in the Snake River Plain aquifer. Representative compressed chromatograms for all ground waters sampled in this study are available on two 3.5-inch high density computer disks. The data and the program required to decompress the data can be obtained from the U.S. Geological Survey office at Idaho Falls, Idaho. Sulfur hexafluoride (SF6) concentrations were measured in selected wells to determine the feasibility of using this environmental tracer as an age dating tool of ground water. Concentrations of dissolved nitrogen, argon, carbon dioxide, oxygen, and methane were measured in 79 ground waters. Concentrations of dissolved permanent gases are tabulated and will be used to evaluate the temperature of recharge of ground water in and near the INEEL.

A comparison of LBW and GTAW processes in miniature closure welds

NASA Astrophysics Data System (ADS)

Knorovsky, G. A.; Fuerschbach, P. W.; Gianoulakis, S. E.; Burchett, S. N.

When small electronic components with glass-to-metal seals are closure welded, the residual stresses that develop in the glass are of concern. If these stresses exceed allowable tensile levels' the resulting weld-induced seal failure may cause the entire component to be scrapped or reworked at a substantial cost. Conventional wisdom says the best welding process for these applications is that which provides the least heat input, and so in that respect, Laser Beam Welding (LBW) provides less heat input than Gas Tungsten Arc Welding (GTAW), however, other concerns, such as weld fit-up, part variability, and material weldability, can modify the final choice of a welding process. In this paper, we compare the characteristic levels of heat input and the residual stresses generated in glass seals for two processes (as calculated by a 3D Finite Element Analysis) as a function of heat input and travel speed, and contrast some of the other manufacturing decisions that must be made in choosing a production process. The geometry chosen is that of a standing edge corner weld in a cylindrical container about 20 mm diameter by 35 mm tall. Four metal pins are glassed into the part lid. The stresses calculated from the resulting from continuous wave CO2 LBW are compared with those resulting from GTAW. The total energy required by the laser weld is significantly less than that needed for the equivalent size GTA weld. The energy input requirements for a given size weld is inversely proportional to the travel speed, but approaches a saturation level as the travel speed increases. LBW travel speeds ranging from 10 mm/s to 50 mm/s were examined.

Reproducible Crystal Growth Experiments in Microgravity Science Glovebox at the International Space Station (SUBSA Investigation)

NASA Technical Reports Server (NTRS)

Ostrogorsky, A.; Marin, C.; Volz, M. P.; Bonner, W. A.

2005-01-01

Solidification Using a Baffle in Sealed Ampoules (SUBSA) is the first investigation conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. 8 single crystals of InSb, doped with Te and Zn, were directionally solidified in microgravity. The experiments were conducted in a furnace with a transparent gradient section, and a video camera, sending images to the earth. The real time images (i) helped seeding, (ii) allowed a direct measurement of the solidification rate. The post-flight characterization of the crystals includes: computed x-ray tomography, Secondary Ion Mass Spectroscopy (SIMS), Hall measurements, Atomic Absorption (AA), and 4 point probe analysis. For the first time in microgravity, several crystals having nearly identical initial transients were grown. Reproducible initial transients were obtained with Te-doped InSb. Furthermore, the diffusion controlled end-transient was demonstrated experimentally (SUBSA 02). From the initial transients, the diffusivity of Te and Zn in InSb was determined.

Multi-Layer SnSe Nanoflake Field-Effect Transistors with Low-Resistance Au Ohmic Contacts

NASA Astrophysics Data System (ADS)

Cho, Sang-Hyeok; Cho, Kwanghee; Park, No-Won; Park, Soonyong; Koh, Jung-Hyuk; Lee, Sang-Kwon

2017-05-01

We report p-type tin monoselenide (SnSe) single crystals, grown in double-sealed quartz ampoules using a modified Bridgman technique at 920 °C. X-ray powder diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX) measurements clearly confirm that the grown SnSe consists of single-crystal SnSe. Electrical transport of multi-layer SnSe nanoflakes, which were prepared by exfoliation from bulk single crystals, was conducted using back-gated field-effect transistor (FET) structures with Au and Ti contacts on SiO2/Si substrates, revealing that multi-layer SnSe nanoflakes exhibit p-type semiconductor characteristics owing to the Sn vacancies on the surfaces of SnSe nanoflakes. In addition, a strong carrier screening effect was observed in 70-90-nm-thick SnSe nanoflake FETs. Furthermore, the effect of the metal contacts to multi-layer SnSe nanoflake-based FETs is also discussed with two different metals, such as Ti/Au and Au contacts.

Study of sealing quality of small {Li}/{SOCl 2} cells

NASA Astrophysics Data System (ADS)

Jian, Tian; Schenzhong, Liu

An examination is made of the sealing of small {Li}/{SOCl 2} cells in a high-temperature condition (200 °C). The metal/metal weld has good quality, but the glass/metal connection between the terminal pin, insulator and the lid is relatively poor. The development of cracks in the insulator, that originate from the Griffith microseam, is due to the combined reaction of temperature, pressure, stress corrosion and bubbles.

Improvement of the lipophilic-oxygen radical absorbance capacity (L-ORAC) method and single-laboratory validation.

PubMed

Watanabe, Jun; Oki, Tomoyuki; Takebayashi, Jun; Yamasaki, Koji; Takano-Ishikawa, Yuko; Hino, Akihiro; Yasui, Akemi

2013-01-01

We improved the procedure for lipophilic-oxygen radical absorbance capacity (L-ORAC) measurement for better repeatability and intermediate precision. A sealing film was placed on the assay plate, and glass vials and microdispensers equipped with glass capillaries were used. The antioxidant capacities of food extracts can be evaluated by this method with nearly the same precision as antioxidant solutions.

A stability-study of expired ampoules manufactured more than 40 years ago.

PubMed

Zilker, Markus; Sörgel, Fritz; Holzgrabe, Ulrike

2018-02-20

Pharmaceutical manufacturers have to study the stability of drug products before marketing according to ICH guideline Q1A(R2); data of those investigations aim to set expiry dates. The expiry date on the container of a remedy assures the physician and the patient a stability of the drug in its formulation i.e. within a specification of 95-105%. Only few studies show that shelf-lives of pharmaceutical products are often longer than expiration dates. The objective of the study presented here was determining the content of nine expired ampoules manufactured in the last century and identifying the impurity profile by means of HPLC-UV and HPLC-MS, respectively. The ampoules are part of the "PEAK-collection" of long expired finished pharmaceutical products at IBMP, Nürnberg-Heroldsberg, and consists among others of epinephrine (Suprarenin and Adrenalin in Oil), etilefrine (Effortil ® ), synephrine (Sympatol ® ), caffeine and procaine (Impletol), caffeine and sodium salicylate (Caffeinum Salicylicum), dipyridamole (Persantin ® ), furosemide (Lasix ® ), and metamizole (Novalgin ® ). For chromatographic investigations methods of the European Pharmacopoeia for related substances were used; for determining the content, they were validated for linearity, precision, and accuracy. The results were compared to current reference ampoules. Five out of nine ampoules were still within the specified content limits. In Suprarenin and Adrenalin in Oil, both containing epinephrine, Impletol (procaine), and Persantin ® (dipyridamole) contents were decreased to 70%, 74%, 79%, and 86%, respectively, and therefore out of specification. Copyright © 2017 Elsevier B.V. All rights reserved.

Simulation of radial solute segregation in vertical Bridgman growth of pyridine-doped benzene, a surrogate for binary organic nonlinear optical materials

NASA Astrophysics Data System (ADS)

Lee, Hanjie; Pearlstein, Arne J.

2000-09-01

We present steady axisymmetric computations of solute distributions and radial segregation for vertical Bridgman growth of pyridine-doped benzene, a binary aromatic system with anisotropic solid-phase thermal conductivity, that serves as a model of solute transport in crystal growth of organic nonlinear optical materials. The radial variation of solid-phase mass fraction ( Cs) of pyridine, which is rejected at the growing interface, depends strongly on growth conditions. High growth velocities tend to increase Cs near the centerline, the ampoule wall, or both, and low growth velocities give more nearly uniform radial distributions. The maximum ampoule-wall temperature gradient also affects radial segregation, with convex-to-the-liquid interfaces at small temperature gradients being associated with radially monotonic Cs distributions, and ridged interfaces at higher gradients being associated with nonmonotonic distributions having maxima at the centerline and ampoule wall. Nonuniformity is strongly determined by both interface shape and the nature of the flow near the interface. Solute is transported down to the interface by a large toroidal vortex, and swept radially inward to the centerline by a second, flattened toroidal cell. When the interface is depressed at its junction with the ampoule wall, rejected solute accumulates in the overlying liquid, where convection is relatively weak, resulting in local solute enrichment of the solid. Computations at normal and zero gravity show that for two very similar interface shapes, a maximum in the radial solid-phase solute distribution at the ampoule wall is associated with the interface shape, while the maximum on the centerline is associated with sweeping of solute to the centerline by a vortical flow on the interface. We also show that radial solute segregation depends significantly on whether account is taken of the anisotropy of the solid-phase thermal conductivity. Finally, the computations provide guidance as to the minimum ampoule length required to produce an axially uniform solute distribution over at least part of the length of a boule.

Li.sub.2 O-Al.sub.2 O.sub.3 -SiO.sub.2 glass ceramic-aluminum containing austenitic stainless steel composite body and a method of producing the same

DOEpatents

Cassidy, Roger T.

1990-05-01

The present invention relates to a hermetically sealed Li.sub.2 O-Al.sub.2 O.sub.3 -SiO.sub.2 glass ceramic-aluminum containing stainless steel composite body and a method of producing the body. The composite body includes an oxide interfacial region between the glass ceramic and metal, wherein the interfacial region consists essentially of an Al.sub.2 O.sub.3 layer. The interfacial Al.sub.2 O.sub.3 region includes constituents of both the metal and glass ceramic.

Helicopter winchmens' experiences with pain management in challenging environments.

PubMed

van der Velde, J; Linehan, L; Cusack, S

2013-02-01

We conducted a survey of Irish Coast Guard Search and Rescue Helicopter winchmen to establish if their pain management scope of practice was adequate for their working environment. We surveyed 17 SAR personnel. 88% of winchmen have experienced scenarios where they were unable to reduce pain scores below 6/10. In seeking solutions within current Irish Prehospital Clinical Practice Guidelines, repeated descriptions of operations in extreme weather and sea conditions were given which were entirely incompatible with the dexterity required to break a glass ampoule and draw up solution, let alone site an intravenous (IV) line or administer a drug via intramuscular (IM) injection. Irish Coast Guard Search and Rescue Helicopter winchmen encounter polytrauma patients in extreme pain in uniquely challenging environments. Novel solutions to pain management within this tightly governed system are urgently required.

Metallic seal for thermal barrier coating systems

NASA Technical Reports Server (NTRS)

Miller, Robert A. (Inventor)

1990-01-01

The invention is particularly concerned with sealing thermal barrier coating systems of the type in use and being contemplated for use in diesel and other internal combustion engines. The invention also would find application in moderately high temperature regions of gas turbine engines and any other application employing a thermal barrier coating at moderate temperatures. Ni-35Cr-6Al-1Y, Ni-35Cr-6Al-1Yb, or other metallic alloy denoted as MCrAlx is applied over a zirconia-based thermal barrier overlayer. The close-out layer is glass-bead preened to densify its surface. This seals and protects the thermal barrier coating system.

49 CFR 173.196 - Category A infectious substances.

Code of Federal Regulations, 2010 CFR

2010-10-01

... the following requirements, depending on the physical state and other characteristics of the material... of glass, metal, or plastic. Positive means of ensuring a leakproof seal must be provided, such as...

Micromolded PDMS planar electrode allows patch clamp electrical recordings from cells.

PubMed

Klemic, Kathryn G; Klemic, James F; Reed, Mark A; Sigworth, Fred J

2002-06-01

The patch clamp method measures membrane currents at very high resolution when a high-resistance 'gigaseal' is established between the glass microelectrode and the cell membrane (Pflugers Arch. 391 (1981) 85; Neuron 8 (1992) 605). Here we describe the first use of the silicone elastomer, poly(dimethylsiloxane) (PDMS), for patch clamp electrodes. PDMS is an attractive material for patch clamp recordings. It has low dielectric loss and can be micromolded (Annu. Rev. Mat. Sci. 28 (1998) 153) into a shape that mimics the tip of the glass micropipette. Also, the surface chemistry of PDMS may be altered to mimic the hydrophilic nature of glass (J. Appl. Polym. Sci. 14 (1970) 2499; Annu. Rev. Mat. Sci. 28 (1998) 153), thereby allowing a high-resistance seal to a cell membrane. We present a planar electrode geometry consisting of a PDMS partition with a small aperture sealed between electrode and bath chambers. We demonstrate that a planar PDMS patch electrode, after oxidation of the elastomeric surface, permits patch clamp recording on Xenopus oocytes. Our results indicate the potential for high-throughput patch clamp recording with a planar array of PDMS electrodes.

Loss of preservative from a tuberculin solution in rubber stoppered vials fastened with different seals.

PubMed

Held, H R; Landi, S

1985-07-01

A tuberculin purified protein derivative (PPD) solution containing 0.3% phenol as a preservative was dispensed in glass vials closed with rubber stoppers fastened in three different ways, namely with Tear-off seals, Flip-off seals and partial seals. After various times of storage at 5 degrees C and 37 degrees C, the phenol content in the tuberculin solution was determined. It was found that the Flip-off seals allowed the phenol to escape at a faster rate than the Tear-off seals and that vials closed with partial seals showed the highest loss of phenol. Although these losses were much more pronounced at 37 degrees C than at 5 degrees C, the phenol content at the latter temperature was, over a period of three years, within the limits of acceptability for tuberculin products capped with Tear-off or Flip-off seals. A loss of phenol also occurred from tuberculin solution stored at -28 degrees C in vials capped with either Tear-off or partial seals. In addition to the Tear-off and Flip-off seals other seals such as the "controlled score' Flip-off seal and the Alcoa Steri-Twist cap were evaluated for their imperviousness to air. Except for the Alcoa Steri-Twist cap none of the seals we have investigated were air tight and hence entirely satisfactory to prevent losses of phenol by evaporation from tuberculin products.(ABSTRACT TRUNCATED AT 250 WORDS)

Inexpensive cryogenic insulation replaces vacuum jacketed line

NASA Technical Reports Server (NTRS)

Fuchs, C. E.

1967-01-01

Commercially available aluminized Mylar, cork and fiber glass form a multilayered sealed system and provide rugged and economical field installed insulation for cryogenic /liquid nitrogen or oxygen/ pipe lines in an exposed environment.

49 CFR 173.13 - Exceptions for Class 3, Divisions 4.1, 4.2, 4.3, 5.1, 6.1, and Classes 8 and 9 materials.

Code of Federal Regulations, 2011 CFR

2011-10-01

... material must be placed in a tightly closed glass, plastic or metal inner packaging with a maximum capacity... placed in a hermetically sealed barrier bag which is impervious to the lading. (v) The intermediate... hazardous material must be placed in a tightly closed glass, plastic or metal inner packaging. The net...

49 CFR 173.13 - Exceptions for Class 3, Divisions 4.1, 4.2, 4.3, 5.1, 6.1, and Classes 8 and 9 materials.

Code of Federal Regulations, 2013 CFR

2013-10-01

... material must be placed in a tightly closed glass, plastic or metal inner packaging with a maximum capacity... placed in a hermetically sealed barrier bag which is impervious to the lading. (v) The intermediate... hazardous material must be placed in a tightly closed glass, plastic or metal inner packaging. The net...

49 CFR 173.13 - Exceptions for Class 3, Divisions 4.1, 4.2, 4.3, 5.1, 6.1, and Classes 8 and 9 materials.

Code of Federal Regulations, 2014 CFR

2014-10-01

... material must be placed in a tightly closed glass, plastic or metal inner packaging with a maximum capacity... placed in a hermetically sealed barrier bag which is impervious to the lading. (v) The intermediate... hazardous material must be placed in a tightly closed glass, plastic or metal inner packaging. The net...

49 CFR 173.13 - Exceptions for Class 3, Divisions 4.1, 4.2, 4.3, 5.1, 6.1, and Classes 8 and 9 materials.

Code of Federal Regulations, 2012 CFR

2012-10-01

... material must be placed in a tightly closed glass, plastic or metal inner packaging with a maximum capacity... placed in a hermetically sealed barrier bag which is impervious to the lading. (v) The intermediate... hazardous material must be placed in a tightly closed glass, plastic or metal inner packaging. The net...

49 CFR 173.13 - Exceptions for Class 3, Divisions 4.1, 4.2, 4.3, 5.1, 6.1, and Classes 8 and 9 materials.

Code of Federal Regulations, 2010 CFR

2010-10-01

... material must be placed in a tightly closed glass, plastic or metal inner packaging with a maximum capacity... placed in a hermetically sealed barrier bag which is impervious to the lading. (v) The intermediate... hazardous material must be placed in a tightly closed glass, plastic or metal inner packaging. The net...

Isothermal dendritic growth experiment: Science, engineering, and hardware development for USMP space flights

NASA Astrophysics Data System (ADS)

Glicksman, M. E.; Hahn, R. C.; Koss, M. B.; Tirmizi, S. H.; Selleck, M. E.; Velosa, A.; Winsa, E.

The Isothermal Dendritic Growth Experiment (IDGE) has been designed to provide microgravity data on dendritic growth for a critical test of theory. This paper updates our progress on constructing a crystal growth chamber suitable for space flight. The IDGE chamber is constructed from glass and stainless steel and is hermetically sealed by electron beam welds and glass-metal seals. Initial tests of the chambers sample's melting point plateau show that the new chamber design is capable of preserving the 99.9995 pct purity of succinonitrile (SCN). One can initiate dendrite growth in the center of the IDGE chamber by means of thermo-electric coolers and a capillary injector tube (stinger). The new IDGE chamber is ready for fully integrated tests with the prototype IDGE engineering hardware at NASA's Lewis Research Center.

Automated method for determining Instron Residual Seal Force of glass vial/rubber closure systems.

PubMed

Ludwig, J D; Nolan, P D; Davis, C W

1993-01-01

Instron Residual Seal Force (IRSF) of glass vial/rubber closure systems was determined using an Instron 4501 Materials Testing System. Computer programs were written to process raw data and calculate IRSF values. Preliminary experiments indicated both the appearance of the stress-deformation curves and precision of the derived IRSF values were dependent on the internal dimensions and top surface geometry of the cap anvil. Therefore, a series of five cap anvils varying in shape and dimensions were machined to optimize performance and precision. Vials capped with West 4416/50 PURCOAT button closures or Helvoet compound 6207 lyophilization closures were tested with each cap anvil. Cap anvils with spherical top surfaces and narrow internal dimensions produced more precise results and more uniform stress-deformation curves than cap anvils with flat top surfaces and wider internal dimensions.

Effect of silane pretreatment on the immediate bonding of universal adhesives to computer-aided design/computer-aided manufacturing lithium disilicate glass ceramics.

PubMed

Yao, Chenmin; Zhou, Liqun; Yang, Hongye; Wang, Yake; Sun, Hualing; Guo, Jingmei; Huang, Cui

2017-04-01

The aim of this study was to investigate the effect of silane pretreatment on the universal adhesive bonding between lithium disilicate glass ceramic and composite resin. IPS e.max ceramic blocks etched with hydrofluoric acid were randomly assigned to one of eight groups treated with one of four universal adhesives (two silane-free adhesives and two silane-containing adhesives), each with or without silane pretreatment. Bonded specimens were stored in water for 24 h. The shear bond strength (SBS) of the ceramic-resin interface was measured to evaluate bond strength, and the debonded interface after the SBS test was analysed using field-emission scanning electron microscopy to determine failure mode. Light microscopy was performed to analyse microleakage and marginal sealing ability. Silane pretreatment significantly and positively influenced SBS and marginal sealing ability. For all the universal adhesive groups, SBS increased and the percentage of microleakage decreased after the pretreatment. Without the pretreatment, SBS and the percentage of microleakage were not significantly different between the silane-containing universal adhesive groups and the silane-free groups. Cohesive failure was the main fracture pattern. The results suggest that additional silane pretreatment can effectively improve the bonding strength and marginal sealing of adhesives to lithium disilicate glass ceramics. The bonding performance of silane-containing universal adhesives without pretreatment is similar to that of silane-free adhesives. © 2017 Eur J Oral Sci.

Hydrothermal transformations in an aluminophosphate glass matrix containing simulators of high-level radioactive wastes

NASA Astrophysics Data System (ADS)

Yudintsev, S. V.; Mal'kovsky, V. I.; Mokhov, A. V.

2016-05-01

The interaction of aluminophosphate glass with water at 95°C for 35 days results in glass heterogenization and in the appearance of a gel layer and various phases. The leaching rate of elements is low owing to the formation of a protective layer on the glass surface. It is shown that over 80% of uranium leached from the glass matrix occurs as colloids below 450 nm in size characterized by high migration ability in the geological environment. To determine the composition of these colloids is a primary task for further studies. Water vapor is a crystallization factor for glasses. The conditions as such may appear even at early stages of glass storage because of the failure of seals on containers of high-level radioactive wastes. The examination of water resistance of crystallized matrices and determination of the fraction of radionuclide in colloids are also subjects for further studies.

Effect of Interface Shape and Magnetic Field on the Microstructure of Bulk Ge:Ga

NASA Technical Reports Server (NTRS)

Cobb, S. D.; Szofran, F. R.; Volz, M. P.

1999-01-01

Thermal and compositional gradients induced during the growth process contribute significantly to the development of defects in the solidified boule. Thermal gradients and the solid-liquid interface shape can be greatly effected by ampoule material. Compositional gradients are strongly influenced by interface curvature and convective flow in the liquid. Results of this investigation illustrate the combined influences of interface shape and convective fluid flow. An applied magnetic field was used to reduce the effects of convective fluid flow in the electrically conductive melt during directional solidification. Several 8 mm diameter boules of Ga-doped Ge were grown at different field strengths, up to 5 Tesla, in four different ampoule materials. Compositional profiles indicate mass transfer conditions ranged from completely mixed to diffusion controlled. The influence of convection in the melt on the developing crystal microstructure and defect density was investigated as a function of field strength and ampoule material. Chemical etching and electron backscattered electron diffraction were used to map the crystal structure of each boule along the center plane. Dislocation etch pit densities were measured for each boule. Results show the influence of magnetic field strength and ampoule material on overall crystal quality.

76 FR 81363 - Temperature-Indicating Devices; Thermally Processed Low-Acid Foods Packaged in Hermetically...

Federal Register 2010, 2011, 2012, 2013, 2014

2011-12-28

... Foods Packaged in Hermetically Sealed Containers; Correction AGENCY: Food and Drug Administration, HHS... containers to allow for use of other temperature-indicating devices, in addition to mercury-in-glass...

Microcracks, micropores, and their petrologic interpretation for 72415 and 15418

NASA Technical Reports Server (NTRS)

Richter, D.; Simmons, G.; Siegfried, R.

1976-01-01

Lunar samples 72415 and 15418 have complex microstructures that indicate a series of fracturing and healing events. Both samples contain relatively few open microcracks but many sealed and healed microcracks. Dunite 72415 contains abundant healed cracks that formed tectonically, symplectic intergrowths spatially and probably genetically related to microcracks, and a cataclastic matrix that has been extensively sintered. Metamorphosed breccia 15418 contains many post-metamorphic healed cracks, large shock induced cracks that have been sealed with glass, and a few younger, thin, open shock induced cracks.

Effect of Water Vapor Pressure on Fatigue Crack Growth in Al-Zn-Cu-Mg Alloy Over Wide-Range Stress Intensity Factor Loading

DTIC Science & Technology

2014-05-07

impacts: (a) crack closure, (b) transport of water vapor molecules within the fatigue crack (47], and (c) tensile stress-plastic strain range...sealed stainless steel UHV chamber. Pure water vapor was introduced from a sealed glass flask containing triply distilled water, via a precision leak...lamellar for H1 flow in a fatigue crack in steel ; specifically, flow is dominated by the low dynamic viscosity of a gas (particularly at low pressures) and

High thermal expansion, sealing glass

DOEpatents

Brow, Richard K.; Kovacic, Larry

1993-01-01

A glass composition for hermetically sealing to high thermal expansion materials such as aluminum alloys, stainless steels, copper, and copper/beryllium alloys, which includes between about 10 and about 25 mole percent Na.sub.2 O, between about 10 and about 25 mole percent K.sub.2 O, between about 5 and about 15 mole percent Al.sub.2 O.sub.3, between about 35 and about 50 mole percent P.sub.2 O.sub.5 and between about 5 and about 15 mole percent of one of PbO, BaO, and mixtures thereof. The composition, which may also include between 0 and about 5 mole percent Fe.sub.2 O.sub.3 and between 0 and about 10 mole percent B.sub.2 O.sub.3, has a thermal expansion coefficient in a range of between about 160 and 210.times.10-7/.degree.C. and a dissolution rate in a range of between about 2.times.10.sup.- 7 and 2.times.10.sup.-9 g/cm.sup.2 -min. This composition is suitable to hermetically seal to metallic electrical components which will be subjected to humid environments over an extended period of time.

High thermal expansion, sealing glass

DOEpatents

Brow, R.K.; Kovacic, L.

1993-11-16

A glass composition is described for hermetically sealing to high thermal expansion materials such as aluminum alloys, stainless steels, copper, and copper/beryllium alloys, which includes between about 10 and about 25 mole percent Na[sub 2]O, between about 10 and about 25 mole percent K[sub 2]O, between about 5 and about 15 mole percent Al[sub 2]O[sub 3], between about 35 and about 50 mole percent P[sub 2]O[sub 5] and between about 5 and about 15 mole percent of one of PbO, BaO, and mixtures thereof. The composition, which may also include between 0 and about 5 mole percent Fe[sub 2]O[sub 3] and between 0 and about 10 mole percent B[sub 2]O[sub 3], has a thermal expansion coefficient in a range of between about 160 and 210[times]10[sup [minus]7]/C and a dissolution rate in a range of between about 2[times]10[sup [minus]7] and 2[times]10[sup [minus]9]g/cm[sup 2]-min. This composition is suitable to hermetically seal to metallic electrical components which will be subjected to humid environments over an extended period of time.

Prototype Rechargeable Lithium Batteries. Phase 1

DTIC Science & Technology

1987-06-01

pentoxide [ V2o5 ], titanium disulfide [TiS ], vanadium V) sulfide [V2S 5 ], and lithium cobalt oxide [Li Co02]) witi high conductivity, ester-Eased...2400 envelope while the cathodes were supported with porous glass disks to maintain good electrical contact with the expanded metal current collectors...cells consisted of an electrode stack mounted between two glass slides held together with stainless steel wire and sealed in a Fisher & Porter 3-ounce

Manufacturing Technology Study on Radio Frequency Power Modules Packaging Techniques.

DTIC Science & Technology

1981-01-01

compromised; in most cases, it was found to be higher than our original process. An accelerated high 125 I temperature aging test was performed to attain...sealing glasses without some oxynen. Alternatively, there are many high temperature amorphous type glasses which satisfactorily fire in nitrogen but...achieve some degree of crystalization when fired at high temperature . In using the high temperatures (900°C range) the effect on the previously printed

[In vitro drug release behavior of carrier made of porous glass ceramics].

PubMed

Wang, De-ping; Huang, Wen-hai; Zhou, Nai

2002-09-01

To conduct the in vitro test on drug release of rifampin encapsulated in a carrier made of porous phosphate glass ceramics and to analyze main factors which affect the drug release rate. A certain quantitative of rifampin was sealed in a hollow cylindrical capsule which consisted of chopped calcium phosphate crystal fiber obtained from glass crystallization. The rifampin concentration was measured in the simulated physiological solution in which the capsule soaked. Rifampin could be released in a constant rate from the porous glass ceramic carrier in a long time. The release rate was dependent on the size of crystal fiber and the wall thickness of the capsule. This kind of calcium phosphate glass ceramics can be a candidate of the carrier materials used as long term drug therapy after osteotomy surgery.

Additive manufacturing of borosilicate glass (Conference Presentation)

NASA Astrophysics Data System (ADS)

Luo, Junjie; Goldstein, Jonathan T.; Urbas, Augustine M.; Bristow, Douglas A.; Landers, Robert G.; Kinzel, Edward C.

2017-02-01

Glasses including have significant scientific and engineering applications including optics, communications, electronics, and hermetic seals. This paper investigates a filament fed process for Additive Manufacturing (AM) of borosilicate glasses. Compared to soda-lime glasses, borosilicate glasses have improved coefficient of thermal expansion (CTE) and are widely used because of thermal shock resistance. In this work, borosilicate glass filaments are fed into a CO2 laser generated melt pool, smoothly depositing material onto the workpiece. Single tracks are printed to explore the effects that different process parameters have on the morphology of printed glass as well as the residual stress trapped in the glass. The transparency of glass allows residual stress to be measured using a polariscope. The effect of the substrate as well and substrate temperature are analyzed. We show that if fracture due to thermal shock can be avoided during deposition, then the residual stress can be relieved with an annealing step, removing birefringence. When combined with progress toward avoiding bubble entrapment in printed glass, we show the AM approach has the potential to produce high quality optically transparent glass for optical applications.

Wavelength properties of DCG holograms under the conditions of different temperature and humidity

NASA Astrophysics Data System (ADS)

Liu, Yujie; Li, Wenqiang; Ding, Quanxin; Yan, Zhanjun

2014-12-01

Holograms recorded in dichromated gelatin (DCG) are usually sealed with a glass plate cemented with an epoxy glue to protect the holograms from moisture in the environment. An investigation of the wavelength properties of sealed DCG holograms had been carried out paying attention to holograms which were exposed to different temperature and humidity environment in this work. The investigation had revealed that (a) exposing the sealed DCG holograms to high relative humidity (RH=98%) environment or immersing them in room-temperature water for 20 hours can not affect the holograms; (b) the sealed DCG holograms can be used at temperature below 50°C without showing undue detrimental effects regarding their optical properties; (c) the peak wavelength of sealed DCG holograms can cause blue shift of several nanometers at 70°C~85°C and the velocity of blue shift is proportional to the environmental temperature; (d) the holograms can be destroyed at 100° or above. The experimental results above will be analyzed and discussed in this paper. A method to improve the stability of sealed DCG holograms is proposed: baking the sealed DCG holograms at proper temperature (e.g., 85°C in this study).

Material Properties of Three Candidate Elastomers for Space Seals Applications

NASA Technical Reports Server (NTRS)

Bastrzyk, Marta B.; Daniels, Christopher C.; Oswald, Jay J.; Dunlap, Patrick H., Jr.; Steinetz, Bruce M.

2010-01-01

A next-generation docking system is being developed by the National Aeronautics and Space Administration (NASA) to support Constellation Space Exploration Missions to low Earth orbit (LEO), to the Moon, and to Mars. A number of investigations were carried out to quantify the properties of candidate elastomer materials for use in the main interface seal of the Low Impact Docking System (LIDS). This seal forms the gas pressure seal between two mating spacecraft. Three candidate silicone elastomer compounds were examined: Esterline ELA-SA-401, Parker Hannifin S0383-70, and Parker Hannifin S0899-50. All three materials were characterized as low-outgassing compounds, per ASTM E595, so as to minimize the contamination of optical and solar array systems. Important seal properties such as outgas levels, durometer, tensile strength, elongation to failure, glass transition temperature, permeability, compression set, Yeoh strain energy coefficients, coefficients of friction, coefficients of thermal expansion, thermal conductivity and diffusivity were measured and are reported herein.

Application of atomic layer deposited microchannel plates to imaging photodetectors with high time resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Siegmund, O. H. W.; McPhate, J. B.; Tremsin, A. S.

Novel microchannel plates have been constructed using borosilicate glass micro-capillary array substrates with 20 mu m and 10 mu m pores and coated with resistive, and secondary electron emissive, layers by atomic layer deposition. Microchannel plates in 33 mm, 50 mm and 20 cm square formats have been made and tested. Although their amplification, imaging, and timing properties are comparable to standard glass microchannel plates, the background rates and lifetime characteristics are considerably improved. Sealed tube detectors based on the Planacon tube, and a 25 mm cross delay line readout tube with a GaN(Mg) opaque photocathode deposited on borosilicate microchannelmore » plates have been fabricated. Considerable progress has also been made with 20 cm microchannel plates for a 20 cm format sealed tube sensor with strip-line readout that is being developed for Cherenkov light detection.« less

Calibration of the NPL secondary standard radionuclide calibrator for 32P, 89Sr and 90Y

NASA Astrophysics Data System (ADS)

Woods, M. J.; Munster, A. S.; Sephton, J. P.; Lucas, S. E. M.; Walsh, C. Paton

1996-02-01

Pure beta particle emitting radionuclides have many therapeutic applications in nuclear medicine. The response of the NPL secondary standard radionuclide calibrator to 32P, 89Sr and 90Y has been measured using accurately calibrated solutions. For this purpose, high efficiency solid sources were prepared gravimetrically from dilute solutions of each radionuclide and assayed in a 4π proportional counter; the source activities were determined using known detection efficiency factors. Measurements were made of the current response (pA/MBq) of the NPL secondary standard radionuclide calibrator using the original concentrated solutions. Calibration figures have been derived for 2 and 5 ml British Standard glass ampoules and Amersham International plc P6 vials. Volume correction factors have also been determined. Gamma-ray emitting contaminants can have a disproportionate effect on the calibrator response and particular attention has been paid to this.

Glass ceramic seals to inconel

DOEpatents

McCollister, Howard L.; Reed, Scott T.

1983-11-08

A glass ceramic composition prepared by subjecting a glass composition comprising, by weight, 65-80% SiO.sub.2, 8-16%, Li.sub.2 O, 2-8% , Al.sub.2 O.sub.3, 1-8% K.sub.2 O, 1-5% P.sub.2 O.sub.5 and 1.5-7% B.sub.2 O.sub.3, to the following processing steps of heating the glass composition to a temperature sufficient to crystallize lithium metasilicate therein, holding the glass composition at a temperature and for a time period sufficient to dissolve the lithium metasilicate therein thereby creating cristobalite nucleii, cooling the glass composition and maintaining the composition at a temperature and for a time period sufficient to recrystallize lithium metasilicate therein, and thermally treating the glass composition at a temperature and for a time period sufficient to cause growth of cristobalite and further crystallization of lithium metasilicate producing a glass ceramic composition having a specific thermal expansion coefficient and products containing said composition.

Glass ceramic-to-metal seals

DOEpatents

Not Available

1982-04-19

A glass ceramic composition prepared by subjecting a glass composition comprising, by weight, 65 to 80% SiO/sub 2/, 8 to 16% Li/sub 2/O, 2 to 8% Al/sub 2/O/sub 3/, 1 to 8% K/sub 2/O, 1 to 5% P/sub 2/O/sub 5/ and 1.5 to 7% B/sub 2/O/sub 3/, to the following processing steps of heating the glass composition to a temperature sufficient to crystallize lithium metasilicate therein, holding the glass composition at a temperature and for a time period sufficient to dissolve the lithium metasilicate therein thereby creating cristobalite nucleii, cooling the glass composition and maintaining the composition at a temperature and for a time period sufficient to recrystallize lithium metasilicate therein, and thermally treating the glass composition at a temperature and for a time period sufficient to caus growth of cristobalite and further crystallization of lithium metasilicate producing a glass ceramic composition having a specific thermal expansion coefficient and products containing said composition.

Numerical modeling of physical vapor transport under microgravity conditions: Effect of thermal creep and stress

NASA Technical Reports Server (NTRS)

Mackowski, Daniel W.; Knight, Roy W.

1993-01-01

One of the most promising applications of microgravity (micro-g) environments is the manufacture of exotic and high-quality crystals in closed cylindrical ampoules using physical vapor transport (PVT) processes. The quality enhancements are believed to be due to the absence of buoyant convection in the weightless environment - resulting in diffusion-limited transport of the vapor. In a typical experiment, solid-phase sample material is initially contained at one end of the ampoule. The sample is made to sublime into the vapor phase and deposit onto the opposite end by maintaining the source at an elevated temperature with respect to the deposit. Identification of the physical factors governing both the rates and uniformity of crystal growth, and the optimization of the micro-g technology, will require an accurate modeling of the vapor transport within the ampoule. Previous micro-g modeling efforts have approached the problem from a 'classical' convective/diffusion formulation, in which convection is driven by the action of buoyancy on thermal and solutal density differences. The general conclusion of these works have been that in low gravity environments the effect of buoyancy on vapor transport is negligible, and vapor transport occurs in a diffusion-limited mode. However, it has been recently recognized than in the non-isothermal (and often low total pressure) conditions encountered in ampoules, the commonly-assumed no-slip boundary condition to the differential equations governing fluid motion can be grossly unrepresentative of the actual situation. Specifically, the temperature gradients can give rise to thermal creep flows at the ampoule side walls. In addition, temperature gradients in the vapor itself can, through the action of thermal stress, lead to bulk fluid convection.

Comparative Study of 14C-Labeled Purified Protein Derivative from Various Mycobacteria

PubMed Central

Landi, S.; Held, H. R.; Tseng, M. C.

1970-01-01

Biologically active 14C-labeled purified protein derivative (14C-PPD) has been prepared from the culture filtrates of seven species of mycobacteria, namely Mycobacterium tuberculosis Johnston strain (PPD), M. bovis BCG (PPD-BCG), M. avium (PPD-A), M. kansasii (PPD-Y), M. intracellulare (PPD-B), M. scrofulaceum (PPD-G), and M. fortuitum (PPD-F). These mycobacteria were grown in a culture medium containing a mixture of 14C-labeled amino acids. The yield and specific radioactivity of the PPD, of the nucleic acid, of the bacterial cells, and of the CO2 developed during growth have been determined for each of the seven species of mycobacteria. Although the yields of 14C-PPD antigens differed greatly for the different species of mycobacteria tested, their specific radioactivities were similar. The 14C-PPD antigens have been used as a means to measure their adsorption to glass. When glass ampoules containing dilute solutions (0.001 mg of PPD per ml) of these PPD antigens (PPD, PPD-BCG, PPD-A, PPD-Y, PPD-G, PPD-B, and PPD-F) were stored for 12 months at 5 C, it was found that they all adsorbed equally well to glass surfaces. In fact, regardless of the origin of the PPD, a loss due to adsorption of about 90% occurred during the first month of storage, and thereafter the PPD content remained practically constant for the rest of the duration of the storage period. The addition of 0.0005% Tween 80 to the PPD solutions effectively reduced the adsorption to glass of most PPD antigens. However, adsorption of PPD-BCG was not quite so effectively prevented, even when the Tween 80 concentration was increased from 0.0005 to 0.0005%. Images PMID:5485082

Cross-Effects in Microgravity Flows

NASA Technical Reports Server (NTRS)

Loyalka, Sudarshan K.; Tompson, R. V.; Ivchenko, I. N.; Ghosh, T. K.; Hamoodi, S. A.; Hickey, K. A.; Huang, C. M.; Tebbe, Patrick A.; Gabis, D. H.; Tekasakul, P.;

SealSim Version 1.1

DOE Office of Scientific and Technical Information (OSTI.GOV)

SealSim 1.1 is a state-of-the-art, Microsoft Windows based computer program developed for the U.S. Department of Energy by Aspen Research Corporation with Contracted support from TNO TPD. It is intended to be used by manufacturers, engineers, educators, students, architects, and others to help determine the relative durability of Insulating Glass Units (IGU). As a function of time, SealSim 1.1 simulates the behaviour of an Insulating Glass Unit, exposed to realistic or user-defined weather climates. Stresses and strains in the IGU are calculated as a function of time, together with temperature distributions, gas permeation effects (gas loss, desiccant loading), dew pointmore » temperature, U-factor, etc. The current version of SealSim 1.1 supports double-glazing Units. where the spacer system is either a Thermo Plastic Spacer (TPS) or Box type spacer. For the determination of solar properties of glazing systems, SealSim 1.1 uses the Tntemational Glazing Database of LBNL, which is also used by OPTICS and WINDOW. The goal of the SealSim 1.1 simulations is to predict the IGU's average lifetime, expressed in terms of the "Durability Index", together with the associated failure mechanisms. The Durability Index of a particular IGU and its most probable failure mechanism can be compared with other IGU's. How the predicted Durability Index relates to the actual durability of an IGU is not known, simply because sufficient experimental data is lacking for describing the behaviour of IG Units over extended periods of time together with a lack of knowledge of the conditions it is subjected to and initial state of the CU at the time of manufacturing. In order to simulate the IGU behaviour in time, the conditions of the IGU must be defined; together with the weather and or climate that the IGU is subjected to. Using physical models of the IGU, SealSim 1.1 calculates tte response of the CU in time. These physical models are described in more detail in separate documents provided with the SealSim 1.1 program. Though much care was taken to test the correct implementation of physical sub models in SealSim 1.1, make the graphical user interface intuitive, making it robust, and to check all options that are available in SealSim 1.1, it will certainly suffer from the deficiencies of a first release. Aspen Research Corporation 1700 Buerkle Road St Paul, Minnesota 55110« less

Utility Distribution Systems in Sweden, Finland, Norway and England

DTIC Science & Technology

1976-11-01

the duct adds to the water protection and sumps, with access for pumping, are provided -at low points. Glass wool or mineral wool insulation is placed...mm thick, is glass, mineral wool or polyurethane foam. The outer pipe is steel, polyurethane or asbestos cement coupled with O-ring seals. Asbestos...decided that asbestos cement should be replaced by less dangerous materials. Some use is made of steel, plastic or copper tubes with mineral wool or

Cryogenic Flange and Seal Evaluation

NASA Technical Reports Server (NTRS)

Ramirez, Adrian

2014-01-01

The assembly of flanges, seals, and pipes are used to carry cryogenic fluid from a storage tank to the vehicle at launch sites. However, after a certain amount of cycles these raised face flanges with glass-filled Teflon gaskets have been found to have torque relaxation and are as a result susceptible to cryogenic fluid leakage if not re-torqued. The intent of this project is to identify alternate combinations of flanges and seals which may improve thermal cycle performance and decrease re-torque requirements. The general approach is to design a test fixture to evaluate leak characteristics between spiral and concentric serrations and to test alternate flange and seal combinations. Due to insufficient time, it was not possible to evaluate these different types of combinations for the combination that improved thermal cycle performance the most. However, the necessary drawings for the test fixture were designed and assembled along with the collection of the necessary parts.

Method for forming hermetic seals

NASA Technical Reports Server (NTRS)

Gallagher, Brian D.

1987-01-01

The firmly adherent film of bondable metal, such as silver, is applied to the surface of glass or other substrate by decomposing a layer of solution of a thermally decomposable metallo-organic deposition (MOD) compound such as silver neodecanoate in xylene. The MOD compound thermally decomposes into metal and gaseous by-products. Sealing is accomplished by depositing a layer of bonding metal, such as solder or a brazing alloy, on the metal film and then forming an assembly with another high melting point metal surface such as a layer of Kovar. When the assembly is heated above the temperature of the solder, the solder flows, wets the adjacent surfaces and forms a hermetic seal between the metal film and metal surface when the assembly cools.

A combined arc-melting and tilt-casting furnace for the manufacture of high-purity bulk metallic glass materials.

PubMed

Soinila, E; Pihlajamäki, T; Bossuyt, S; Hänninen, H

2011-07-01

An arc-melting furnace which includes a tilt-casting facility was designed and built, for the purpose of producing bulk metallic glass specimens. Tilt-casting was chosen because reportedly, in combination with high-purity processing, it produces the best fatigue endurance in Zr-based bulk metallic glasses. Incorporating the alloying and casting facilities in a single piece of equipment reduces the amount of laboratory space and capital investment needed. Eliminating the sample transfer step from the production process also saves time and reduces sample contamination. This is important because the glass forming ability in many alloy systems, such as Zr-based glass-forming alloys, deteriorates rapidly with increasing oxygen content of the specimen. The challenge was to create a versatile instrument, in which high purity conditions can be maintained throughout the process, even when melting alloys with high affinity for oxygen. Therefore, the design provides a high-vacuum chamber to be filled with a low-oxygen inert atmosphere, and takes special care to keep the system hermetically sealed throughout the process. In particular, movements of the arc-melting electrode and sample manipulator arm are accommodated by deformable metal bellows, rather than sliding O-ring seals, and the whole furnace is tilted for tilt-casting. This performance of the furnace is demonstrated by alloying and casting Zr(55)Cu(30)Al(10)Ni(5) directly into rods up to ø 10 mm which are verified to be amorphous by x-ray diffraction and differential scanning calorimetry, and to exhibit locally ductile fracture at liquid nitrogen temperature.

Ampule tests to simulate glass corrosion in ambient temperature lithium batteries. Volume 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Douglas, S.C.; Bunker, B.C.; Crafts, C.C.

1984-06-01

Glass corrosion in battery headers has been found to limit the shelf life of ambient temperature lithium batteries. Glass corrosion can lead to loss of battery electrolytes or to shorts across the conductive corrosion product. Tests have been conducted which simulate the corrosive environment in a battery by sealing headers attached to lithium metal into Pyrex ampules containing battery electrolyte. Using the ampule test, glass corrosion kinetics have been determined at 70/sup 0/C for the Li/SO/sub 2/, Li/SOCl/sub 2/, and Li/SOCl/sub 2/ + BrCl battery systems. Test results indicate that corrosion of commercial glass compositions is extensive in all electrolytesmore » tested, resulting in predicted battery failures after several months. Sandia's TA-23 glass corrodes at a much slower rate, indicating a projected battery lifetime of over five years in the Li/SO/sub 2/ system. Test results reveal that corrosion kinetics are sensitive to header polarization, stress, and configuration as well as glass composition.« less

Hermetic encapsulation technique for solar arrays

NASA Technical Reports Server (NTRS)

Deminet, C.; Horne, W. E.

1980-01-01

A concept is presented for encapsulating solar cells between two layers of glass either individually, in panels, or in a continuous process. The concept yields an integral unit that is hermetically sealed and that is tolerant to high temperature thermal cycling and to particulate radiation. Data are presented on both high temperature solar cells and special glasses that soften at low temperatures for use with the concept. The results of encapsulating experiments are presented which show the successful application of the concept to the special high temperature cells. The mechanical feasibility of encapsulating 2 mil cells between two layers of 2 mil glass is also demonstrated.

Ceramic sealants prepared by polymer pyrolysis

NASA Astrophysics Data System (ADS)

Hong, Sung Jin; Kim, Deug Joong; Yoo, Young Sung

2011-02-01

The formation and properties of ceramic seals for SOFC applications prepared by polymer pyrolysis are investigated. A mixture with polymethylsiloxane and fillers are pyrolyzed in a N2 atmosphere. The coefficient of thermal expansion of the ceramic composites was controlled by fillers with a high coefficient of thermal expansion such as AlCo. The morphology of the ceramic composites derived from the mixture with polymethylsiloxane and fillers is composed of fillers embedded in a Si-O-C glass matrix. The thermal expansion behavior and sealing characteristics are measured and discussed

Study on influence of growth conditions on position and shape of crystal/melt interface of alkali lead halide crystals at Bridgman growth

NASA Astrophysics Data System (ADS)

Král, Robert

2012-12-01

Suitable conditions for growth of high quality single crystals of ternary alkali lead halides prepared by a Bridgman method were explored using direct observation of a crystal/melt interface when pulling an ampoule out of a furnace, deliberated striations' induction and measurement of a temperature field in the filled ampoule in the vertical Bridgman arrangement, as model compounds lead chloride and ternary rubidium lead bromide were used. By direct observation only position of the crystal/melt interface was markedly determined, while by induced striations both the position and the shape of the interface were visualized but their contrast had to be intensified by adding admixtures. Performed temperature measurements in the filled ampoule brought both a view of temperature field in the 3D radial symmetry and basic data for comparison of a real temperature field with those obtained by projected modeling.

Shock Reactivity of Non-Porous Mixtures of Manganese and Sulfur

NASA Astrophysics Data System (ADS)

Jetté, F. X.; Goroshin, S.; Higgins, A. J.

2007-12-01

Equimolar mixtures of manganese powder and sulfur were melt-cast into solid pellets in order to study the mechanism of shock-enhanced reactivity in non-porous heterogeneous mixtures. This mixture was selected due to the large exothermic heat release of the manganese-sulfur reaction (214 kJ/mol), which causes the reaction to be self-sustaining once initiated. The test samples were placed in planar recovery ampoules and a strong shock was delivered via the detonation of a charge of amine-sensitized nitromethane. Various shock strengths were achieved by placing different thicknesses of PMMA attenuator discs between the explosive charge and the ampoule. The results confirmed that shock-induced reactions can be produced in highly non-porous mixtures. Indeed, the critical shock pressure that caused ignition of the mixture in the ampoule was found to be in the range 2.2-3.0 GPa (pressures were estimated using LS-DYNA simulations of samples with 100% TMD).

Astronaut Peggy Whitson Installs SUBSA Experiment

NASA Technical Reports Server (NTRS)

2002-01-01

Expedition Five flight engineer Peggy Whitson is shown installing the Solidification Using a Baffle in Sealed Ampoules (SUBSA) experiment in the Microgravity Science Glovebox (MSG) in the Destiny laboratory aboard the International Space Station (ISS). SUBSA examines the solidification of semiconductor crystals from a melted material. Semiconductor crystals are used for many products that touch our everyday lives. They are found in computer chips, integrated circuits, and a multitude of other electronic devices, such as sensors for medical imaging equipment and detectors of nuclear radiation. Materials scientists want to make better semiconductor crystals to be able to further reduce the size of high-tech devices. In the microgravity environment, convection and sedimentation are reduced, so fluids do not remove and deform. Thus, space laboratories provide an ideal environment of studying solidification from the melt. This investigation is expected to determine the mechanism causing fluid motion during production of semiconductors in space. It will provide insight into the role of the melt motion in production of semiconductor crystals, advancing our knowledge of the crystal growth process. This could lead to a reduction of defects in semiconductor crystals produced in space and on Earth.

International Space Station (ISS)

NASA Image and Video Library

2002-07-05

Expedition Five flight engineer Peggy Whitson is shown installing the Solidification Using a Baffle in Sealed Ampoules (SUBSA) experiment in the Microgravity Science Glovebox (MSG) in the Destiny laboratory aboard the International Space Station (ISS). SUBSA examines the solidification of semiconductor crystals from a melted material. Semiconductor crystals are used for many products that touch our everyday lives. They are found in computer chips, integrated circuits, and a multitude of other electronic devices, such as sensors for medical imaging equipment and detectors of nuclear radiation. Materials scientists want to make better semiconductor crystals to be able to further reduce the size of high-tech devices. In the microgravity environment, convection and sedimentation are reduced, so fluids do not remove and deform. Thus, space laboratories provide an ideal environment of studying solidification from the melt. This investigation is expected to determine the mechanism causing fluid motion during production of semiconductors in space. It will provide insight into the role of the melt motion in production of semiconductor crystals, advancing our knowledge of the crystal growth process. This could lead to a reduction of defects in semiconductor crystals produced in space and on Earth.

Benzil: 2-methyl-4-nitroaniline binary single crystals for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Choi, Jaeho; Aggarwal, Mohan D.; Wang, Wen Shan; Penn, Benjamin G.; Frazier, Donald O.

1999-06-01

Benzil:MNA binary organic single crystals have been grown to overcome decomposition tendency and improve mechanical properties of 2-methyl-4-nitroaniline (MNA) which is known to be one of the best organic NLO material. Single crystals of binary system have grown using a transparent Bridgman- Stockbarger system which has fabricated to monitor the growth process. The growth conditions for the flat solid- liquid interface are optimized for the different dopant concentration of benzil. The melt in the self-sealing ampoule is maintained in liquid state without decomposition up to 2 weeks which allows us to grow 20 mm long single crystals. Hardness of 5wt% benzil:MNA is measured to be 13 Kg/mm2 which is 45% higher than benzil. The conversion efficiency of second-harmonic generation is found to be 1.5% with 4.5 mm interaction length. Since MNA is phase-matchable material, this efficiency could be comparable to commercial KDP. Surface quality of binary crystals has maintained its initial condition in air without absorption of water vapor which may be the main cause of surface degradation.

Prevention of chinosol absorption by rubber stoppers used to seal glass vials containing tuberculin PPD Mantoux solutions.

PubMed

Landi, S; Held, H R

1965-01-01

Chinosol (8-quinolinol sulfate), which is employed as an antimicrobial agent in tuberculin PPD solutions used for the Mantoux test, is known to disappear from these solutions after storage. It has been established that the loss of this preservative from tuberculin solutions dispensed in glass vials is caused by the rubber stoppers used to seal the vials. All the rubber stoppers tested absorbed Chinosol very readily.The nature of the binding of Chinosol by a rubber stopper is both chemical (irreversible) and physical (reversible). The capacity to bind Chinosol chemically was determined for 12 types of rubber stopper, and was found to vary from 0 to more than 25% by weight of the stopper. This phenomenon can be attributed mainly to metal ingredients in the stopper. The capacity of stoppers to bind Chinosol physically is expressed quantitatively by a partition coefficient. This was determined for 7 types of rubber stopper and found to be high when compared with the partition coefficients of other preservatives.We have shown that all stoppers presaturated in Chinosol can be equilibrated against a buffered solution containing 0.01% Chinosol. Equilibrated silicone, white, and red oxiglazed stoppers can be used satisfactorily for sealing multi-dose vials of tuberculin PPD containing 0.01% Chinosol.

Prevention of Chinosol absorption by rubber stoppers used to seal glass vials containing tuberculin PPD Mantoux solutions

PubMed Central

Landi, S.; Held, H. R.

1965-01-01

Chinosol (8-quinolinol sulfate), which is employed as an antimicrobial agent in tuberculin PPD solutions used for the Mantoux test, is known to disappear from these solutions after storage. It has been established that the loss of this preservative from tuberculin solutions dispensed in glass vials is caused by the rubber stoppers used to seal the vials. All the rubber stoppers tested absorbed Chinosol very readily. The nature of the binding of Chinosol by a rubber stopper is both chemical (irreversible) and physical (reversible). The capacity to bind Chinosol chemically was determined for 12 types of rubber stopper, and was found to vary from 0 to more than 25% by weight of the stopper. This phenomenon can be attributed mainly to metal ingredients in the stopper. The capacity of stoppers to bind Chinosol physically is expressed quantitatively by a partition coefficient. This was determined for 7 types of rubber stopper and found to be high when compared with the partition coefficients of other preservatives. We have shown that all stoppers presaturated in Chinosol can be equilibrated against a buffered solution containing 0.01% Chinosol. Equilibrated silicone, white, and red oxiglazed stoppers can be used satisfactorily for sealing multi-dose vials of tuberculin PPD containing 0.01% Chinosol. ImagesFIG. 2 PMID:5294923

Research support for cadmium telluride crystal growth

NASA Technical Reports Server (NTRS)

Rosenberger, Franz

1995-01-01

The growth of single crystals of zinc selenide was carried out by both closed ampoule physical vapor transport and effusive ampoule physical vapor transport (EAPVT). The latter technique was shown to be a much more efficient method for the seeded growth of zinc selenide, resulting in higher transport rates. Furthermore, EAPVT work on CdTe has shown that growth onto (n 11) seeds is advantageous for obtaining reduced twinning and defect densities in II-VI sphalerite materials.

Effect of V2O5 on SrO-ZnO-B2O3-SiO2 glass-ceramics for high temperature sealant application

NASA Astrophysics Data System (ADS)

Tiwari, Babita; Bhatacharya, S.; Dixit, A.; Gadkari, S. C.; Kothiyal, G. P.

2012-06-01

Glasses in the SrO-ZnO-B2O3-SiO2 (SZBS) system with and without V2O5 were prepared by melt-quench method and transformed into glass-ceramics by controlled crystallization. Investigated glasses and glass-ceramics have thermal expansion coefficients (TEC) in the range of 95-120 × 10-7/°C (30-600 °C), which match closely with TEC of other components of solid oxide fuel cell (SOFC). Study of thermo-physical properties of SZBS glasses revealed the network modifying effect of V2O5. Addition of V2O5 increases the TEC and decreases the viscosity of the glass which is beneficial for making seal with Crofer-22-APU. Microstructural investigations have shown good bonding of SZBS glasses with Crofer-22-APU. Elemental line scans indicate that inter-diffusion of Fe, Cr and Si across interface, which is thought to be responsible for good bonding with Crofer-22-APU.

Novel hermetic packaging methods for MOEMS

NASA Astrophysics Data System (ADS)

Stark, David

2003-01-01

Hermetic packaging of micro-optoelectromechanical systems (MOEMS) is an immature technology, lacking industry-consensus methods and standards. Off-the-shelf, catalog window assemblies are not yet available. Window assemblies are in general custom designed and manufactured for each new product, resulting in longer than acceptable cycle times, high procurement costs and questionable reliability. There are currently two dominant window-manufacturing methods wherein a metal frame is attached to glass, as well as a third, less-used method. The first method creates a glass-to-metal seal by heating the glass above its Tg to fuse it to the frame. The second method involves first metallizing the glass where it is to be attached to the frame, and then soldering the glass to the frame. The third method employs solder-glass to bond the glass to the frame. A novel alternative with superior features compared to the three previously described window-manufacturing methods is proposed. The new approach lends itself to a plurality of glass-to-metal attachment techniques. Benefits include lower temperature processing than two of the current methods and potentially more cost-effective manufacturing than all three of today"s attachment methods.

Lipid bilayer mechanics in a pipette with glass-bilayer adhesion.

PubMed

Ursell, Tristan; Agrawal, Ashutosh; Phillips, Rob

2011-10-19

Electrophysiology is a central tool for measuring how different driving forces (e.g., ligand concentration, transmembrane voltage, or lateral tension) cause a channel protein to gate. Upon formation of the high resistance seal between a lipid bilayer and a glass pipette, the so-called "giga-seal", channel activity can be recorded electrically. In this article, we explore the implications of giga-seal formation on the mechanical state of a lipid bilayer patch. We use a mechanical model for the free energy of bilayer geometry in the presence of glass-bilayer adhesion to draw three potentially important conclusions. First, we use our adhesion model to derive an explicit relationship between applied pressure and patch shape that is consistent with the Laplace-Young Law, giving an alternative method of calculating patch tension under pressure. With knowledge of the adhesion constant, which we find to be in the range ∼0.4-4 mN/m, and the pipette size, one can precisely calculate the patch tension as a function of pressure, without the difficultly of obtaining an optical measurement of the bilayer radius of curvature. Second, we use data from previous electrophysiological experiments to show that over a wide range of lipids, the resting tension on a electrophysiological patch is highly variable and can be 10-100 times higher than estimates of the tension in a typical cell membrane. This suggests that electrophysiological experiments may be systematically altering channel-gating characteristics and querying the channels under conditions that are not the same as their physiological counterparts. Third, we show that reversible adhesion leads to a predictable change in the population response of gating channels in a bilayer patch. Copyright © 2011 Biophysical Society. Published by Elsevier Inc. All rights reserved.

Noninvasive pit and fissure sealing: microtensile bond strength to intact bovine enamel of different pit and fissure sealants in a simplified fissure model.

PubMed

Papacchini, Federica; Cury, Alvaro H; Goracci, Cecilia; Chieffi, Nicoletta; Tay, Franklin R; Polimeni, Antonella; Ferrari, Marco

2006-12-01

To measure the microtensile bond strength of different pit and fissure sealants in a simplified fissure model. Twenty extracted bovine mandibular permanent incisors were randomly divided into 4 groups for treatment: G1: 35% phosphoric acid/Clinpro Sealant; G2: 35% phosphoric acid/Delton; G3: Non-Rinse Conditioner/Dyract Seal; G4: 20% polyacrylic acid/Fuji IILC. Each tooth was sectioned into 6 pieces (4 x 6 mm) of buccal enamel. SEM examination was used to confirm the presence of aprismatic enamel on each tooth. Using a spacer, two pieces of etched enamel were secured to a glass slide at a mean distance of 0.6+/-0.1 mm. The space between enamel substrates was then etched/conditioned and sealed with different materials according to the tested groups. By serially cutting each double-bonded sample, multiple beam-shaped specimens about 0.8mm(2) in cross section were obtained and tested in tension (0.5 mm/min) until failure occurred at either one of the two stressed interfaces. Failure modes were classified by stereomicroscopy. G1 and G2 showed statistically higher bond strengths than G3 and G4. G4 demonstrated the significantly lowest bond strength. Failures were mostly adhesive in G1, G2, G3, and mainly cohesive/mixed in G4. According to this model, resin-based materials (Clinpro Sealant, Delton) showed better microtensile bond strength than compomer (Dyract Seal) or resin-modified glass ionomer (Fuji IILC).

Gold nano-particle formation from crystalline AuCN: Comparison of thermal, plasma- and ion-beam activated decomposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Beck, Mihály T.; Bertóti, Imre, E-mail: bertoti.imre@ttk.mta.hu; Mohai, Miklós

In this work, in addition to the conventional thermal process, two non-conventional ways, the plasma and ion beam activations are described for preparing gold nanoparticles from microcrystalline AuCN precursor. The phase formation at plasma and ion beam treatments was compared with that at thermal treatments and the products and transformations were characterized by thermogravimetry-mass-spectrometry (TG-MS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). TG-MS measurements in Ar atmosphere revealed that AuCN decomposition starts at 400 °C and completes at ≈700 °C with evolution of gaseous (CN){sub 2}. XPS and TEM show that in heat treatment at 450 °C formore » 1 h in Ar, loss of nitrogen and carbon occurs and small, 5–30 nm gold particles forms. Heating at 450 °C for 10 h in sealed ampoule, much larger, 60–200 nm size and well faceted Au particles develop together with a fibrous (CN){sub n} polymer phase, and the Au crystallites are covered by a 3–5 nm thick polymer shell. Low pressure Ar plasma treatment at 300 eV energy results in 4–20 nm size Au particles and removes most of the nitrogen and part of carbon. During Ar{sup +} ion bombardment with 2500 eV energy, 5–30 nm size Au crystallites form already in 10 min, with preferential loss of nitrogen and with increased amount of carbon residue. The results suggest that plasma and ion beam activation, acting similarly to thermal treatment, may be used to prepare Au nanoparticles from AuCN on selected surface areas either by depositing AuCN precursors on selected regions or by focusing the applied ionized radiation. Thus they may offer alternative ways for preparing tailor-made catalysts, electronic devices and sensors for different applications. - Graphical abstract: Proposed scheme of the decomposition mechanism of AuCN samples: heat treatment in Ar flow (a) and in sealed ampoule (b); Ar{sup +} ion treatment at 300 eV (c) and at 2500 eV (d). Cross section sketches illustrate the Au phase formation and the corresponding TEM micrographs are shown as top views. The dotted lines represent the original boundaries of the AuCN crystals. - Highlights: • AuCN decomposes between 400 and 700 °C with evolution of gaseous (CN){sub 2}. • Epitaxial relationship is established between Au and parent AuCN crystals. • Ar plasma treatment results in similar phase transition than the thermal treatment. • Plasma and ion-beam activation offer alternative way for preparing Au nanocrystals. • Reaction mechanisms of Au particle formation at the three treatments are proposed.« less

Suppression of span in sealed microcavity Fabry-Perot pressure sensors

NASA Astrophysics Data System (ADS)

Mishra, Shivam; Rajappa, Balasubramaniam; Chandra, Sudhir

2017-01-01

Optical microelectromechanical system pressure sensors working on the principle of extrinsic Fabry-Perot (FP) interferometer are designed and fabricated for pressure range of 1-bar absolute. Anodic bonding of silicon with glass is performed under atmospheric pressure to form FP cavity. This process results in entrapment of gas in the sealed microcavity. The effect of trapped gas is investigated on sensor characteristics. A closed-loop solution is derived for the deflection of the diaphragm of a sealed microcavity pressure sensor. Phenomenon of "suppression of span" is brought out. The sensors are tested using white light interferometry technique. The residual pressure of the trapped gas is estimated from the experiments. The developed model has been used to estimate the deflection sensitivity of the free diaphragm and the extent of suppression of span after bonding.

30 CFR 20.8 - Class 1 lamps.

Code of Federal Regulations, 2011 CFR

2011-07-01

... glass is accidentally broken, and ignition by electric sparks or arcs from the battery or connections... other than flashlights, all parts, such as bulb housing and battery container, through which access may... made for sealing the battery container. (4) Battery current restricted. Unless all current-carrying...

30 CFR 20.8 - Class 1 lamps.

Code of Federal Regulations, 2013 CFR

2013-07-01

... glass is accidentally broken, and ignition by electric sparks or arcs from the battery or connections... other than flashlights, all parts, such as bulb housing and battery container, through which access may... made for sealing the battery container. (4) Battery current restricted. Unless all current-carrying...

30 CFR 20.8 - Class 1 lamps.

Code of Federal Regulations, 2012 CFR

2012-07-01

... glass is accidentally broken, and ignition by electric sparks or arcs from the battery or connections... other than flashlights, all parts, such as bulb housing and battery container, through which access may... made for sealing the battery container. (4) Battery current restricted. Unless all current-carrying...

30 CFR 20.8 - Class 1 lamps.

Code of Federal Regulations, 2014 CFR

2014-07-01

... glass is accidentally broken, and ignition by electric sparks or arcs from the battery or connections... other than flashlights, all parts, such as bulb housing and battery container, through which access may... made for sealing the battery container. (4) Battery current restricted. Unless all current-carrying...

Determining Kinetic Parameters for Isothermal Crystallization of Glasses

NASA Technical Reports Server (NTRS)

Ray, C. S.; Zhang, T.; Reis, S. T.; Brow, R. K.

2006-01-01

Non-isothermal crystallization techniques are frequently used to determine the kinetic parameters for crystallization in glasses. These techniques are experimentally simple and quick compared to the isothermal techniques. However, the analytical models used for non-isothermal data analysis, originally developed for describing isothermal transformation kinetics, are fundamentally flawed. The present paper describes a technique for determining the kinetic parameters for isothermal crystallization in glasses, which eliminates most of the common problems that generally make the studies of isothermal crystallization laborious and time consuming. In this technique, the volume fraction of glass that is crystallized as a function of time during an isothermal hold was determined using differential thermal analysis (DTA). The crystallization parameters for the lithium-disilicate (Li2O.2SiO2) model glass were first determined and compared to the same parameters determined by other techniques to establish the accuracy and usefulness of the present technique. This technique was then used to describe the crystallization kinetics of a complex Ca-Sr-Zn-silicate glass developed for sealing solid oxide fuel cells.

Constitutive Modeling of a Glass Fiber-Reinforced PTFE Gasketed-Joint Under a Re-torque

NASA Astrophysics Data System (ADS)

Williams, James; Gordon, Ali P.

Joints gasketed with viscoelastic seals often receive an application of a secondary torque, i.e., retorque, in order to ensure joint tightness and proper sealing. The motivation of this study is to characterize and analytically model the load and deflection re-torque response of a single 25% glass-fiber reinforced polytetrafluorethylene (PTFE) gasket-bolted joint with serrated flange detail. The Burger-type viscoelastic modeling constants of the material are obtained through isolating the gasket from the bolt by performing a gasket creep test via a MTS electromechanical test frame. The re-load creep response is also investigated by re-loading the gasket after a period of initial creep to observe the response. The modeling constants obtained from the creep tests are used with a Burger-type viscoelastic model to predict the re-torque response of a single bolt-gasket test fixture in order to validate the ability of the model to simulate the re-torque response under various loading conditions and flange detail.

Growth of zinc selenide crystals by physical vapor transport in microgravity

NASA Technical Reports Server (NTRS)

Rosenberger, Franz

1995-01-01

The growth of single crystals of zinc selenide was carried out by both closed ampoule physical vapor transport and effusive ampoule physical vapor transport (EAPVT). The latter technique was shown to be a much more efficient method for the seeded growth of zinc selenide, resulting in higher transport rates. Furthermore, EAPVT work on CdTe has shown that growth onto /n11/ seeds is advantageous for obtaining reduced twinning and defect densities in II-VI sphalerite materials.

Modelling crystal growth: Convection in an asymmetrically heated ampoule

NASA Technical Reports Server (NTRS)

Alexander, J. Iwan D.; Rosenberger, Franz; Pulicani, J. P.; Krukowski, S.; Ouazzani, Jalil

1990-01-01

The objective was to develop and implement a numerical method capable of solving the nonlinear partial differential equations governing heat, mass, and momentum transfer in a 3-D cylindrical geometry in order to examine the character of convection in an asymmetrically heated cylindrical ampoule. The details of the numerical method, including verification tests involving comparison with results obtained from other methods, are presented. The results of the study of 3-D convection in an asymmetrically heated cylinder are described.

Microleakage of adhesive restorative materials.

PubMed

Gladys, S; Van Meerbeek, B; Lambrechts, P; Vanherle, G

2001-06-01

To compare the marginal sealing ability of two conventional and one polyacid-modified resin-based composite, and two conventional and three resin-modified glass-ionomers in conventional cylindrical box cavities following a silver-staining microleakage evaluation method. In 80 freshly extracted and caries-free human third molars, three standardized cylindrical butt-joint cavities were prepared: the first cavity in coronal enamel, the second at the cemento-enamel junction (CEJ) and the third completely in root cementum. A control group of 10 additional teeth was chosen. After the cavities were restored randomly using the eight restorative materials tested, the specimens were first stored in distilled water at 37 degrees C for 7 days and then thermocycled (500 cycles). Thereafter, the specimens were centrifuged for 10 min in plastic bottles containing 50 wt% silver nitrate aqueous solution. The degree of microleakage was recorded at four different depths along the restoration margins using an optical stereomicroscope equipped with a measuring gauge. None of the tested systems prevented microleakage completely, but the extent of leakage decreased towards the bottom of the restorations. The resin-modified glass-ionomers performed better than the conventional resin-based composites and conventional glass-ionomers. Distinct leakage patterns were recorded among all materials investigated. Complete marginal sealing could still not be reached with the new adhesive restorative materials.

An electrochemical pumping system for on-chip gradient generation.

PubMed

Xie, Jun; Miao, Yunan; Shih, Jason; He, Qing; Liu, Jun; Tai, Yu-Chong; Lee, Terry D

2004-07-01

Within the context of microfluidic systems, it has been difficult to devise pumping systems that can deliver adequate flow rates at high pressure for applications such as HPLC. An on-chip electrochemical pumping system based on electrolysis that offers certain advantages over designs that utilize electroosmotic driven flow has been fabricated and tested. The pump was fabricated on both silicon and glass substrates using photolithography. The electrolysis electrodes were formed from either platinum or gold, and SU8, an epoxy-based photoresist, was used to form the pump chambers. A glass cover plate and a poly(dimethylsiloxane) (PDMS) gasket were used to seal the chambers. Filling of the chambers was accomplished by using a syringe to inject liquid via filling ports, which were later sealed using a glass cover plate. The current supplied to the electrodes controlled the rate of gas formation and, thus, the resulting fluid flow rate. At low backpressures, flow rates >1 microL/min have been demonstrated using <1 mW of power. Pumping at backpressures as high as 200 psi have been demonstrated, with 20 nL/min having been observed using <4 mW. By integrating two electrochemical pumps with a polymer electrospray nozzle, we have confirmed the successful generation of a solvent gradient via a mass spectrometer.

A two-step sealing-and-reinforcement SU8 bonding paradigm for the fabrication of shallow microchannels

NASA Astrophysics Data System (ADS)

Mehboudi, Aryan; Yeom, Junghoon

2018-03-01

Adhesive bonding is a key technique to create microfluidic devices when two separate substrates are used to form microchannels. Among many adhesives explored in microchannel fabrication, SU8 has been widely used as an adhesive layer for sealing the microchannel sidewalls. The majority of the available SU8-based bonding methods, however, suffer from the difficulties associated with sealing of two important types of the microchannel architecture: (1) shallow microchannels with small patterns on a large area, and (2) microchannels with ultra-low aspect ratios (e.g. 6 mm in width and 2~μ m in height). In this paper, a new bonding paradigm based upon the low-temperature and low-pressure SU8 bonding, consisting of two steps of sealing using a thin-SU8-coated PET film and bonding reinforcement using a SU8-coated glass slide, is proposed to resolve the aforementioned difficulties. Since it does not need complicated instruments such as a wafer bonding machine and a lamination device, the developed bonding paradigm is convenient and economical. We successfully demonstrate the compatibility of the proposed bonding paradigm with the two microchannel fabrication approaches based on the glass wet etching and the SU8 photo-lithography, where small microchannels with the innermost surfaces fully made of SU8 are obtained. A theoretical model is employed to better investigate the flow characteristics and the structural behavior of the microchannel including the PET film deformation, strain and von Mises stress distributions, bonding strength, etc. Moreover, we demonstrate the fabrication of the multi-height deep-shallow microchannel sidewalls and their sealing using the SU8-coated PET film. Finally, as a proof-of-concept device, a microfluidic filter consisting of the double-height deep-shallow microchannel is fabricated for separation of 3 µm and 10 µm particles.

Mechanical-structural investigation of chemical strengthening aluminosilicate glass through introducing phosphorus pentoxide

NASA Astrophysics Data System (ADS)

Zeng, Huidan; Wang, Ling; Ye, Feng; Yang, Bin; Chen, Jianding; Chen, Guorong; Sun, Luyi

2016-11-01

Chemical strengthening of aluminosilicate glasses through K+-Na+ ion exchange has attracted tremendous attentions because of the accelerating demand for high strength and damage resistance glasses. However, a paramount challenge still exists to fabricate glasses with a higher strength and greater depth of ion-exchange layer. Herein, aluminosilicate glasses with different contents of P2O5 were prepared and the influence of P2O5 on the increased compressive stress and depth of ion-exchange layer was investigated by micro-Raman technique. It was noticed that the hardness, compressive stress, as well as the depth of ion-exchange layer substantially increased with an increasing concentration of P2O5 varied from 1 to 7 mol%. The obtained micro-Raman spectra confirmed the formation of relatively depolymerized silicate anions that accelerated the ion exchange. Phosphorus containing aluminosilicate glasses with a lower polymerization degree exhibited a higher strength and deeper depth of ion-exchange layer, which suggests that the phosphorus containing aluminosilicate glasses have promising applications in flat panel displays, windshields, and wafer sealing substrates.

GEODE 2: Manufacturing large area format cadmium-mercury-telluride crystals in a microgravity environment. Pressure sensor proof of concept

NASA Astrophysics Data System (ADS)

Gale, M. R.; Beattie, D. A.

In the GEODE 1 experiment, a semiconductor Cd-Hg telluride crystal was grown in the MASER1 sounding rocket. It was shown that bulk-quench Cd-Hg telluride crystallization in a microgravity environment results in a more homogeneous crystal structure than can be achieved terrestrially. In the GEODE 2 program, the wall thickness of the quartz ampoule containing the crystal will be reduced to improve the heat transfer characteristics during crystallization. Ampoule explosion must be prevented by active control of the pressure surrounding the weaker, thin-walled ampoule to match that inside the furnace. A prototype pressure sensor that uses the absorption of ultraviolet light by Hg vapor has been built and tested. Pressures from 4 to 40 atmospheres have been measured with a resolution better than 0.35 atmospheres over the entire range. The feasibility of the pressure measurement technique has been demonstrated, although some design improvements are required in order to make measurements more repeatable.

[Thermal resistance of the spores of a Bac. stearothermophilus culture used for the preparation of bioindicators].

PubMed

Kalinina, N M; Shilova, S V; Motina, G L; Chaĭkovskaia, S M

1982-02-01

Thermostability of the spores of Bac. stearothermophilus in ampoules and capillaries in concentrations of 10(9), 10(8) and 10(6) cells per 1 ml of sodium chloride isotonic solution was determined at 119 to 124 degrees C with an interval of 1 degree C and an exposure time of 5, 10, 15, 20, 25, 30, 35 and 40 minutes. The results were used for plotting the survival curves. The time of the microbial death in the ampoules and capillaries at all the temperatures was the same and the ampoules were chosen as the bioindicator vehicle because of their availability and convenience in exploitation. The survival curves may be used for determination of the optimal sterilization conditions. The spore concentration of the thermostable culture in the bioindicator should be equal or exceed the level of the object microbial contamination. In the present study the concentration of the test microbe spores in the bioindicator was 10(6)--10(8) cells/ml.

Multi-ampoule Bridgman growth of halide scintillator crystals using the self-seeding method

NASA Astrophysics Data System (ADS)

Lindsey, Adam C.; Wu, Yuntao; Zhuravleva, Mariya; Loyd, Matthew; Koschan, Merry; Melcher, Charles L.

2017-07-01

We investigate the multi-ampoule growth at 25 mm diameter of ternary iodide single crystal scintillator KCaI3:Eu using the randomly oriented self-seeded Bridgman method. We compare scintillation performance between cubic inch scale crystals containing small variations of low nominal europium concentrations previously shown to balance light yield with self-absorption in the host crystal. Growth conditions were optimized in the developmental furnace and four 2 in3 KCaI3:Eu crystals were grown simultaneously producing a total of six 25 mm × 25 mm cylinders. Small variations in activator concentration did not result in significant performance differences among the six measured crystals. A range of energy resolutions of 3.5-4.7% at 662 keV was achieved, surpassing that of NaI:Tl crystals commonly used in spectroscopic detection applications. The function and basic design of the multi-ampoule furnace as well as the process of growing single crystals of KCaI3 is included here.

Ocean foam generation and modeling

NASA Technical Reports Server (NTRS)

Porter, R. A.; Bechis, K. P.

1976-01-01

A laboratory investigation was conducted to determine the physical and microwave properties of ocean foam. Special foam generators were designed and fabricated, using porous glass sheets, known as glass frits, as the principal element. The glass frit was sealed into a water-tight vertical box, a few centimeters from the bottom. Compressed air, applied to the lower chamber, created ocean foam from sea water lying on the frit. Foam heights of 30 cm were readily achieved, with relatively low air pressures. Special photographic techniques and analytical procedures were employed to determine foam bubble size distributions. In addition, the percentage water content of ocean foam was determined with the aid of a particulate sampling procedure. A glass frit foam generator, with pore diameters in the range 70 - 100 micrometers, produced foam with bubble distributions very similar to those found on the surface of natural ocean foam patches.

The Electronic Structure and Field Effects of an Organic-Based Room Temperature Magnetic Semiconductor

DTIC Science & Technology

2007-01-01

used. Other materials used in this study include: microscope slide glass for transistor substrates (Gold Seal), silicon nitride, Si3N4, sputtering...with the top in place. At LBNL the glass tubes were placed in a nitrogen filled glove bag attached to the XAS sample chamber where they were...valences such as vanadium(II) oxide (VO), vanadium(III) oxide (V2O3), vanadium(IV) oxide (VO2), and vanadium(IV) oxide ( V2O5 ). V2O3 in particular is an

Solar reflection panels

DOEpatents

Diver, Jr., Richard B.; Grossman, James W [Albuquerque, NM; Reshetnik, Michael [Boulder, CO

2006-07-18

A solar collector comprising a glass mirror, and a composite panel, wherein the back of the mirror is affixed to a front surface of the composite panel. The composite panel comprises a front sheet affixed to a surface of a core material, preferably a core material comprising a honeycomb structure, and a back sheet affixed to an opposite surface of the core material. The invention may further comprise a sealing strip, preferably comprising EPDM, positioned between the glass mirror and the front surface of the composite panel. The invention also is of methods of making such solar collectors.

Microleakage of Glass Ionomer-based Provisional Cement in CAD/CAM-Fabricated Interim Crowns: An in vitro Study.

PubMed

Farah, Ra'fat I; Al-Harethi, Naji

2016-10-01

The aim of this study was to compare in vitro the marginal microleakage of glass ionomer-based provisional cement with resin-based provisional cement and zinc oxide non-eugenol (ZONE) provisional cement in computer-aided design and computer-aided manufacturing (CAD/CAM)-fabricated interim restorations. Fifteen intact human premolars were prepared in a standardized manner for complete coverage of crown restorations. Interim crowns for the prepared teeth were then fabricated using CAD/CAM, and the specimens were randomized into three groups of provisional cementing agents (n = 5 each): Glass ionomer-based provisional cement (GC Fuji TEMP LT™), bisphenol-A-glycidyldimethacrylate (Bis-GMA)/ triethylene glycol dimethacrylate (TEGDMA) resin-based cement (UltraTemp® REZ), and ZONE cement (TempBond NE). After 24 hours of storage in distilled water at 37°C, the specimens were thermocycled and then stored again for 24 hours in distilled water at room temperature. Next, the specimens were placed in freshly prepared 2% aqueous methylene blue dye for 24 hours and then embedded in autopolymerizing acrylic resin blocks and sectioned in buccolingual and mesiodistal directions to assess dye penetration using a stereomicroscope. The results were statistically analyzed using a nonparametric Kruskal-Wallis test. Dunn's post hoc test with a Bonferroni correction test was used to compute multiple pairwise comparisons that identified differences among groups; the level of significance was set at p < 0.05. All groups exhibited marginal microleakage; the Bis-GMA/TEGDMA resin-based provisional cement demonstrated the lowest microleakage scores, which were statistically different from those of the glass ionomer-based provisional cement and the ZONE cement. The provisional cementing agents exhibited different sealing abilities. The Bis-GMA/TEGDMA resin-based provisional cement exhibited the most effective favorable sealing properties against dye penetration compared with the glass ionomer-based provisional cement and conventional ZONE cement. Newly introduced glass ionomer-based provisional cement proved to be inferior to resin-based provisional cement as far as marginal microleakage is concerned.

The Effect of Microgravity on the Growth of Lead Tin Telluride

NASA Technical Reports Server (NTRS)

Narayanan, R.

2000-01-01

The main objective of this research was to present a model for the prediction of the effect of the microgravity environment on the growth of Lead Tin Telluride. The attitude change and its relation to the experimental objectives: The main objective for the AADSF experiment on USMP 3 involving LTT growth was to estimate the effect of ampoule orientation on the axial and radial segregation of tin telluride. As the furnace was not situated on a gimbal there was no possibility to reorient the ampoule during the flight. Instead the only way to change the growth orientation was to change the attitude of the orbiter. This was accomplished by vernier rocket firings. In what follows it must be noted that the orbiter body coordinates are such that the positive z axis points outward from the 'belly', the positive 'x' axis points outwards from the nose and the positive 'y' axis points outwards from the starboard side. The furnace which was in the pay load had its axis aligned with the orbiter's 'z' axis with the hot end closest to the shuttle body. There were basically three orientations that were desired. These corresponded to the ampoule being seen as a heated from above (thermally stable-solutally unstable) configuration, the heated from below (where the instabilities were reversed from the first orientation) configuration and an 'in between' case where the ampoule axis was misaligned with respect to the orbiters 'g(sub z)' axis.

Evaluation of a single cell and candidate materials with high water content hydrogen in a generic solid oxide fuel cell stack test fixture, Part II: materials and interface characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chou, Y. S.; Stevenson, Jeffry W.; Choi, Jung-Pyung

2013-01-01

A generic solid oxide fuel cell (SOFC) test fixture was developed to evaluate candidate materials under realistic conditions. A commerical 50 mm x 50 mm NiO-YSZ anode supported thin YSZ electrolyte cell with lanthanum strontium manganite (LSM) cathode was tested to evaluate the stability of candidate materials. The cell was tested in two stages at 800oC: stage I of low (~3% H2O) humidity and stage II of high (~30% H2O) humidity hydrogen fuel at constant voltage or constant current mode. Part I of the work was published earlier with information of the generic test fixture design, materials, cell performance, andmore » optical post-mortem analysis. In part II, detailed microstructure and interfacial characterizations are reported regarding the SOFC candidate materials: (Mn,Co)-spinel conductive coating, alumina coating for sealing area, ferritic stainless steel interconnect, refractory sealing glass, and their interactions with each other. Overall, the (Mn,Co)-spinel coating was very effective in minimizing Cr migration. No Cr was identified in the cathode after 1720h at 800oC. Aluminization of metallic interconnect also proved to be chemically compatible with alkaline-earth silicate sealing glass. The details of interfacial reaction and microstructure development are discussed.« less

New side-view imaging technique for observing posterior chamber structures during cataract surgery in porcine eyes

PubMed Central

2013-01-01

Background To develop a side-view imaging technique for observing the dynamic behavior of posterior chamber structures (PCSs) in porcine eyes which mimics closed-eye cataract surgery in humans. Methods Enucleated porcine eyes were placed into liquid nitrogen for 5 seconds and immediately bisected at about a 45-degree angle to the equatorial plane. The anterior portion was attached firmly to a glass slide with superglue and sprinkled with wheat flour. Phacoemulsification and aspiration (PEA) was performed as in humans on 10 consecutive porcine eyes. The movements of the PCSs were monitored through the glass slide with a high-resolution video camera set below the cut surface of the eye. The intraocular pressure (IOP) was monitored during the surgery. The highest IOP, operation time, and volume of irrigation fluid of 10 whole eyes were compared to that obtained from the bisected eyes glued to a glass slide. In a second set of experiments, the strength of the seal between the bisected eye and the glass slide was tested in three sets of eyes: 1) frozen eye fixed with superglue with wheat flour for 3 min; 2) frozen eye fixed with superglue for 3 min; and 3) non-frozen eye fixed with superglue for 30 min. The highest IOP that led to a disruption of the seal was compared among the three groups. Results PEA was successfully performed on 9 of 10 (90%) eyes with the movements of the PCSs clearly observed. The average maximum intraocular pressure of the 9 bisected eyes was 55.8 ± 4.7 mmHg and that for the 10 unbisected eyes was 55.3 ± 5.0 mmHg (P = 0.650). The frozen eye fixed with superglue in combination with wheat flour (Group 1) had the strongest sealing strength with an average IOP at the breaking point of 117.3 ± 36.2 mmHg. Conclusions Our side-view imaging technique can be used to evaluate the changes of the PCSs during intraocular surgery and for surgical training of new residents. PMID:24053470

Radon gas, useful for medical purposes, safely fixed in quartz

NASA Technical Reports Server (NTRS)

Fields, P. R.; Stein, L.; Zirin, M. H.

1966-01-01

Radon gas is enclosed in quartz or glass ampules by subjecting the gas sealed at a low pressure in the ampules to an ionization process. This process is useful for preparing fixed radon sources for radiological treatment of malignancies, without the danger of releasing radioactive gases.

Method of making nanostructured glass-ceramic waste forms

DOEpatents

Gao, Huizhen; Wang, Yifeng; Rodriguez, Mark A.; Bencoe, Denise N.

2012-12-18

A method of rendering hazardous materials less dangerous comprising trapping the hazardous material in nanopores of a nanoporous composite material, reacting the trapped hazardous material to render it less volatile/soluble, sealing the trapped hazardous material, and vitrifying the nanoporous material containing the less volatile/soluble hazardous material.

Immigration Control: A New Role for the Social Security Card.

DTIC Science & Technology

1988-03-01

aid alterations Yellow. pink, and blue planchettes (discs) No sensory - Very time-consuming for a imeplanted in a random pattern on front and aid...with a magnifying glass counterfeiters, cannot replicate this effect HHS seal blue planchettes , and the words Sensory aid Fluorescent inks not Social

High process yield rates of thermoplastic nanofluidic devices using a hybrid thermal assembly technique.

PubMed

Uba, Franklin I; Hu, Bo; Weerakoon-Ratnayake, Kumuditha; Oliver-Calixte, Nyote; Soper, Steven A

2015-02-21

Over the past decade, thermoplastics have been used as alternative substrates to glass and Si for microfluidic devices because of the diverse and robust fabrication protocols available for thermoplastics that can generate high production rates of the desired structures at low cost and with high replication fidelity, the extensive array of physiochemical properties they possess, and the simple surface activation strategies that can be employed to tune their surface chemistry appropriate for the intended application. While the advantages of polymer microfluidics are currently being realized, the evolution of thermoplastic-based nanofluidic devices is fraught with challenges. One challenge is assembly of the device, which consists of sealing a cover plate to the patterned fluidic substrate. Typically, channel collapse or substrate dissolution occurs during assembly making the device inoperable resulting in low process yield rates. In this work, we report a low temperature hybrid assembly approach for the generation of functional thermoplastic nanofluidic devices with high process yield rates (>90%) and with a short total assembly time (16 min). The approach involves thermally sealing a high T(g) (glass transition temperature) substrate containing the nanofluidic structures to a cover plate possessing a lower T(g). Nanofluidic devices with critical feature sizes ranging between 25-250 nm were fabricated in a thermoplastic substrate (T(g) = 104 °C) and sealed with a cover plate (T(g) = 75 °C) at a temperature significantly below the T(g) of the substrate. Results obtained from sealing tests revealed that the integrity of the nanochannels remained intact after assembly and devices were useful for fluorescence imaging at high signal-to-noise ratios. The functionality of the assembled devices was demonstrated by studying the stretching and translocation dynamics of dsDNA in the enclosed thermoplastic nanofluidic channels.

Manufacture of high-density ceramic sinters

NASA Technical Reports Server (NTRS)

Hibata, Y.

1986-01-01

High density ceramic sinters are manufactured by coating premolded or presintered porous ceramics with a sealing material of high SiO2 porous glass or nitride glass and then sintering by hot isostatic pressing. The ceramics have excellent abrasion and corrosion resistances. Thus LC-10 (Si3N2 powder) and Y2O3-Al2O3 type sintering were mixed and molded to give a premolded porous ceramic (porosity 37%, relative bulk density 63%). The ceramic was dipped in a slurry containing high SiO2 porous glass and an alcohol solution of cellulose acetate and dried. The coated ceramic was treated in a nitrogen atmosphere and then sintered by hot isostatic pressing to give a dense ceramic sinter.

Glass Coats For Hot Isostatic Pressing

NASA Technical Reports Server (NTRS)

Ecer, Gunes M.

1989-01-01

Surface voids sealed from pressurizing gas. Coating technique enables healing of surface defects by hot isostatic pressing (HIP). Internal pores readily closed by HIP, but surface voids like cracks and pores in contact with pressurizing gas not healed. Applied to casting or weldment as thick slurry of two glass powders: one melts at temperature slightly lower than used for HIP, and another melts at higher temperature. For example, powder is glass of 75 percent SiO2 and 25 percent Na2O, while other powder SiO2. Liquid component of slurry fugitive organic binder; for example, mixture of cellulose acetate and acetone. Easy to apply, separates voids from surrounding gas, would not react with metal part under treatment, and easy to remove after pressing.

Investigation of surface tension phenomena using the KC-135 aircraft

NASA Technical Reports Server (NTRS)

Alter, W. S.

1982-01-01

The microgravity environment of the KC-135 aircraft was utilized in three experiments designed to determine the following: (1) the feasibility of measuring critical wetting temperatures; (2) the effectiveness of surface tension as a means of keeping the cushioning heat transfer liquid in the furnace during ampoule translation; and (3) whether a non-wetting fluid would separate from the ampoule wall under low gravity conditions. This trio of investigations concerning surface phenomena demonstrates the effectiveness of the KC-135 as a microgravity research environment for small-scale, hand-held experiments.

Spectrometric investigation of the weathering process affecting historical glasses of León Cathedral, Spain

NASA Astrophysics Data System (ADS)

Castro, M. A.; Pereira, F. J.; Aller, A. J.; Littlejohn, D.

2014-12-01

Atmospheric pollution plays important roles in the weathering of the historical buildings and glass windows. Samples of white powdered weathering products, recovered during restoration of the stained-glass windows of León Cathedral in Spain, were characterised using a combination of scanning electron microscopy (SEM) with energy dispersive-X ray spectrometry (ED-XRS), Fourier transform-infrared (FT-IR) spectroscopy and Raman spectrometry. The presence of sulphates, and to a lesser extent carbonates, in the white powdered product is clear indication of the participation of atmospheric acidifying gases, particularly SOx, in the weathering process. It is interesting to note that there was no indication of the participation of NOx gases. There was, however, evidence that the putty and mortar used to seal/join the glasses were major sources of the weathering products. In this way, this study suggests sealants more resistant to oxidation, such as silicone- and zirconia-based materials, should be considered for repairing glass windows in historic buildings to avoid exacerbating degradation.

Development of Cu(In,Ga)Se2 Test Coupons for Potential Induced Degradation Studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Contreras, Miguel A.; Hacke, Peter; Repins, Ingrid

We report on the design, fabrication and accelerated testing of fully encapsulated small area coupons (approximately 7.5cm x 7.5 cm) for the purpose of researching potential induced degradation in Cu(In, Ga)Se2 based PV modules. The fabrication of these coupons enables the study of the solar cells and the materials used in PV module manufacturing such as top and bottom glass covers of different composition (soda-lime glass, high temperature glass, alkaline-free glass, etc), plastic-based top covers, ethylene vinyl acetate and edge seal encapsulation materials. The coupons can also be used to emulate framed and frameless modules that utilize either monolithically interconnectedmore » modules or singular cell type of modules. The design of the coupons, their fabrication, the materials used and their testing for 1000 hours under 85 degrees C and 85% RH conditions are presented.« less

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Volz, M. P.; Schweizer, M.; Kaiser, N.; Cobb, S. D.; Motakef, S.; Vujisic, L. J.; Croell, A.; Dold, P.; Rose, M. Franklin (Technical Monitor)

2001-01-01

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS) to differentiate among proposed mechanisms contributing to detachment. Sessile drop measurements were first carried out for a large number of substrates made of potential ampoule materials to determine the contact angles and the surface tension as a function of temperature and composition. The process atmosphere and duration of the experiment (for some cases) were also found to have significant influence on the wetting angle. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases to an equilibrium value with duration of measurement ranging from 150 to 117 deg (Ge), 129 to 100 deg (GeSi). Forming gas (Ar + 2% H2) and vacuum have been used in the growth ampoules. With gas in the ampoule, a variation of the temperature profile during growth has been used to control the pressure difference between the top of the melt and the volume below the melt caused by detachment of the growing crystal. The stability of detachment has been modeled and substantial insight has been gained into the reasons that detachment has most often been observed in reduced gravity but nonetheless has occurred randomly even there. An empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed and will be presented. Methods for determining the nature and extent of detachment include profilometry and optical and electron microscopy. This surface study is the subject of another presentation at this Congress. Results in this presentation will show that we have established the effects of different ampoule materials, temperature profiles, pressure differences, and silicon concentrations and that samples that are nearly completely detached can be grown repeatedly.

Numerical Modeling of Physical Vapor Transport in Contactless Crystal Growth Geometry

NASA Technical Reports Server (NTRS)

Palosz, W.; Lowry, S.; Krishnam, A.; Przekwas, A.; Grasza, K.

1998-01-01

Growth from the vapor under conditions of limited contact with the walls of the growth ampoule is beneficial for the quality of the growing crystal due to reduced stress and contamination which may be caused by interactions with the growth container. The technique may be of a particular interest for studies on crystal growth under microgravity conditions: elimination of some factors affecting the crystal quality may make interpretation of space-conducted processes more conclusive and meaningful. For that reason, and as a part of our continuing studies on 'contactless' growth technique, we have developed a computational model of crystal growth process in such system. The theoretical model was built, and simulations were performed using the commercial computational fluid dynamics code, (CFD) ACE. The code uses an implicit finite volume formulation with a gray discrete ordinate method radiation model which accounts for the diffuse absorption and reflection of radiation throughout the furnace. The three-dimensional model computes the heat transfer through the crystal, quartz, and gas both inside and outside the ampoule, and mass transport from the source to the crystal and the sink. The heat transport mechanisms by conduction, natural convection, and radiation, and mass transport by diffusion and convection are modeled simultaneously and include the heat of the phase transition at the solid-vapor interfaces. As the thermal boundary condition, temperature profile along the walls of the furnace is used. For different thermal profiles and furnace and ampoule dimensions, the crystal growth rate and development of the crystal-vapor and source-vapor interfaces (change of the interface shape and location with time) are obtained. Super/under-saturation in the ampoule is determined and critical factors determining the 'contactless' growth conditions are identified and discussed. The relative importance of the ampoule dimensions and geometry, the furnace dimensions and its temperature, and the properties of the grown material are analyzed. The results of the simulations are compared with related experimental results on growth of CdTe, CdZnTe, ZnTe, PbTe, and PbSnTe crystals by this technique.

Semiconducting icosahedral boron arsenide crystal growth for neutron detection

NASA Astrophysics Data System (ADS)

Whiteley, C. E.; Zhang, Y.; Gong, Y.; Bakalova, S.; Mayo, A.; Edgar, J. H.; Kuball, M.

2011-03-01

Semiconducting icosahedral boron arsenide, B12As2, is an excellent candidate for neutron detectors, thermoelectric converters, and radioisotope batteries, for which high quality single crystals are required. Thus, the present study was undertaken to grow B12As2 crystals by precipitation from metal solutions (nickel) saturated with elemental boron (or B12As2 powder) and arsenic in a sealed quartz ampoule. B12As2 crystals of 10-15 mm were produced when a homogeneous mixture of the three elements was held at 1150 °C for 48-72 h and slowly cooled (3.5 °C/h). The crystals varied in color and transparency from black and opaque to clear and transparent. X-ray topography (XRT), and elemental analysis by energy dispersive X-ray spectroscopy (EDS) confirmed that the crystals had the expected rhombohedral structure and chemical stoichiometry. The concentrations of residual impurities (nickel, carbon, etc.) were low, as measured by Raman spectroscopy and secondary ion mass spectrometry (SIMS). Additionally, low etch-pit densities (4.4×107 cm-2) were observed after etching in molten KOH at 500 °C. Thus, the flux growth method is viable for growing large, high-quality B12As2 crystals.

Reconstruction of perfect ZnO nanowires facets with high optical quality

NASA Astrophysics Data System (ADS)

Zehani, E.; Hassani, S.; Lusson, A.; Vigneron, J.; Etcheberry, A.; Galtier, P.; Sallet, V.

2017-07-01

ZnO nanowires were grown on sapphire substrates using metalorganic chemical vapor deposition. The samples were subsequently annealed under zinc pressure in a vacuum-sealed ampoule, at temperature ranging from 500 to 800 °C. The originality and the main motivation to provide a zinc-rich atmosphere were to prevent the out-diffusion of zinc from the nanowires. In doing so, the perfect structural properties and the morphology of the nanowires are kept. Interestingly, photoluminescence experiments performed on nanowires annealed in a narrow window of temperature [580-620 °C] show a spectacular improvement of the optical quality, as transitions commonly observable in high quality bulk samples are found. In addition, the intensity of the so-called "surface excitons" (SX) is strongly decreased. To accurately investigate the chemical modifications of the surface, XPS experiments were carried out and show that zinc hydroxide species and/or Zn(OH)2 sublayer were partially removed from the surface. These results suggest that the annealing process in zinc vapor helps to properly reconstruct the surface of ZnO nanowires, and improves the optical quality of their core. Such a thermal treatment at moderate temperature should be beneficial to nanodevices involving surface reaction, e.g. gas sensors.

Hydrogen-enhanced clusterization of intrinsic defects and impurities in silicon

NASA Astrophysics Data System (ADS)

Mukashev, B. N.; Abdullin, Kh. A.; Gorelkinskii, Yu. V.; Tamendarov, M. F.; Tokmoldin, S. Zh

2001-01-01

Formation of intrinsic and impurity defect complexes in hydrogenated monocrystalline silicon is studied. Hydrogen was incorporated into samples by different ways: either by proton implantation at 80 and 300 K, or by annealing at 1250°C for 30-60 min in a sealed quartz ampoule containing ∼10 -3 ml of distilled water, or by treatment in hydrogen plasma. Radiation defects were incorporated either during the hydrogen implantation or by additional irradiation with protons or α-particles. The measurements were performed by electron paramagnetic resonance (EPR), deep level transient spectroscopy (DLTS) and infrared absorption (IR) methods. Essential differences of defect formation processes in hydrogenated samples as compared with reference samples were detected. The main reasons responsible for the differences are (i) hydrogen precipitation in a supersaturated solution during thermal treatment; (ii) interaction of hydrogen with defects and impurities and hydrogen-induced formation of defects; (iii) ability of hydrogen to play the role of accelerator of impurities precipitation. These factors result in the formation of vacancy-related, interstitial-related and impurity clusters which are observed only in the presence of hydrogen. The nature of the clusters and possible models of their structure are discussed.

Method and apparatus for testing surface characteristics of a material

NASA Technical Reports Server (NTRS)

Johnson, David L. (Inventor); Kersker, Karl D. (Inventor); Stratton, Troy C. (Inventor); Richardson, David E. (Inventor)

2006-01-01

A method, apparatus and system for testing characteristics of a material sample is provided. The system includes an apparatus configured to house the material test sample while defining a sealed volume against a surface of the material test sample. A source of pressurized fluid is in communication with, and configured to pressurize, the sealed volume. A load applying apparatus is configured to apply a defined load to the material sample while the sealed volume is monitored for leakage of the pressurized fluid. Thus, the inducement of surface defects such as microcracking and crazing may be detected and their effects analyzed for a given material. The material test samples may include laminar structures formed of, for example, carbon cloth phenolic, glass cloth phenolic, silica cloth phenolic materials or carbon-carbon materials. In one embodiment the system may be configured to analyze the material test sample while an across-ply loading is applied thereto.

A Simple and Low-Cost Ultramicroelectrode Fabrication and Characterization Method for Undergraduate Students

ERIC Educational Resources Information Center

Sur, Ujjal Kumar; Dhason, A.; Lakshminarayanan, V.

2012-01-01

A laboratory experiment is described in which students fabricate disk-shaped gold and platinum microelectrodes with diameters of 10-50 [mu]m by sealing sodalime glass with metal microwires. The electrodes are characterized by performing cyclic voltammetry in aqueous and acetonitrile solution. Commercial microelectrodes are expensive (cost depends…

Glass-to-Metal Seal Quality.

DTIC Science & Technology

1982-05-01

SELECTION AND EVALUATION . . . . . . . . . . . . . . 2 2.2 MICROELECTRONIC PACKAGES AND THEIR QUALITY . . . * . . . . . . . . 5 2.3 EQUIPMENT...liquid penetrant testing for various microelectronic package hermeticity. I t I MATERIALS AND EQUIPMENT 2.1 DYE PENETRANT SELECTION AND EVALUATION...a commercial visible dye penetrant and a commercial fluorescent dye penetrant were selected as being suitable for the testing of microelectronic

Electrodeless discharge lamp is easily started, has high stability

NASA Technical Reports Server (NTRS)

Bell, W. E.; Bloom, A. L.

1966-01-01

Electrodeless discharge borosilicate glass lamp is used in various high-resolution optical systems. It is partially charged with krypton, contains small amounts of rubidium, and is enclosed in a hermetically sealed envelope that maintains the lamp at an optimum temperature during discharge. The lamp is quickly started by its excitation coil.

The Effect of the Wall Contact and Post-Growth C001-Down on Defects in CdTe Crystals Grown by Contactless PVT

NASA Technical Reports Server (NTRS)

Palosz, W.; Grasza, K.; Dudley, M.; Raghothamachar, B.; Cai, L.; Durose, K.; Halliday, D.; Boyall, N. M.; Rose, M. Franklin (Technical Monitor)

2001-01-01

In crystal growth, the quality of the final material may depend, among other factors, on its interaction with the walls of the ampoule during and after the growth, and on the rate of the crystal cool-down at the end of ate the process. To investigate the above phenomena, a series of CdTe crystal growth processes was carried out, The crystals were grown by physical vapor transport without contact with the side walls of the silica glass ampoules, applying the Low Supersaturation Nucleation technique. The source temperature was 930 C, the undercooling was a few degrees. The crystals, having the diameter of 25 mm, grew at the rate of a few mm per day. The post-growth cool-down to the room temperature was conducted at different rates, and lasted from a few minutes to four days. The crystals were characterized using chemical etching low temperature luminescence, and Synchrotron White Beam X-ray Topography techniques. The dislocation (etch pit) density was measured and its distribution was analyzed by comparison with Poisson curves and with the Normalized Radial Distribution Correlation Function. It was found that the contact of the crystal with silica leads to a strain field and high (in the 105 sq cm range) dislocation (etch pit) density. Similar defect concentrations were found in crystals subjected to fast post-growth cool-down. Typical EPD values for lower cool-down rates and in regions not affected by wall interactions are in the lower 10(exp 4) sq cm range. In some areas the actual dislocation density was about 10(exp 3) sq cm or even less. No apparent effect of the cool-down rate on polygonization was observed. A fine structure could be discerned in low-temperature PL spectra of crystals with low dislocation density.

Solid-State Sensor and Actuator Workshop Held at Hilton Head Island, South Carolina on June 6-9, 1988

DTIC Science & Technology

1988-01-01

Stable Photoresist’, Polym. Figure 71 Eng. Sci. 26 1101(1986) 2) W.E. Feely, " Microplastic Structures, SPIE 631 48(1986) Figure 12 15 A Miniature...unhulbt k- beanils than i ntrini fl t iilins. polys5tilicin sea led cavities fo r re’.i t rain~d uc cr arrays," in Technical Die I IFF IFDN1 p 2;3. I...the The experience with thermal sealing indicates that glass. Sufficient charge transfer occurs to allow th, sea . of glass to metl form when tile metal

Glass for sealing lithium cells

DOEpatents

Leedecke, C.J.

1981-08-28

Glass compositions resistant to corrosion by lithium cell electrolyte and having an expansion coefficient of 45 to 85 x 10/sup -70/C/sup -1/ have been made with SiO/sub 2/, 25 to 55% by weight; B/sub 2/O/sub 3/, 5 to 12%; Al/sub 2/O/sub 3/, 12 to 35%; CaO, 5 to 15%; MgO, 5 to 15%; SrO, 0 to 10%; and La/sub 2/O/sub 3/, 0 to 5%. Preferred compositions within that range contain 3 to 8% SrO and 0.5 to 2.5% La/sub 2/O/sub 3/.

Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

NASA Technical Reports Server (NTRS)

Ritter, T. M.; Volz, M. P.; Cobb, S. D.; Szofran, F. R.

1999-01-01

Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

Study of surface passivation as a function of InP closed-ampoule solar cell fabrication processing variables

NASA Technical Reports Server (NTRS)

Faur, Mircea; Faur, Maria; Jenkins, Phillip; Goradia, Manju; Goradia, Chandra; Bailey, Sheila; Weinberg, Irving; Jayne, Douglas

1990-01-01

The effects of various surface preparation procedures, including chemical treatment and anodic or chemical oxidation, closed-ampoule diffusion conditions, and post-diffusion surface preparation and annealing conditions, on the passivating properties of InP have been investigated in order to optimize the fabrication procedures of n(+)p InP solar cells made by closed-ampoule diffusion of sulfur into p-type InP. The InP substrates used were p-type Cd-doped to a level of 1.7 x 10 to the 16th/cu cm, Zn-doped to levels of 2.2 x 10 to the 16th and 1.2 x 10 to the 18th/cu cm, and n-type S-doped to 4.4 x 10 to the 18th/cu cm. The passivating properties have been evaluated from photoluminescence (PL) and conductance-voltage (G-V) data. Good agreement was found between the level of surface passivation and the composition of different surface layers as revealed by X-ray photoelectron spectroscopy (XPS) analysis.

Fiber optic assembly and method of making same

DOEpatents

Kramer, D.P.; Beckman, T.M.

1997-09-02

There is provided an assembly having a light guiding medium sealed to a holder. Preferably the holder is a metal shell and a light guiding medium is an optical fiber of glass or sapphire whisker. The assembly includes a sealing medium which sealingly engages the metal holder to the fiber. In the formation of the assembly, the seal is essentially hermetic having a capability of minimizing leakage having a helium leak rate of less than 1{times}10{sup {minus}8} cubic centimeters per second and high strength having a capability of withstanding pressures of 100,000 psi or greater. The features of the assembly are obtained by a specific preparation method and by selection of specific starting materials. The fiber is selected to have a sufficiently high coefficient of thermal expansion which minimizes strains in the component during fabrication, as a result of fabrication, and during use. The other components are selected to be of a material having compatible coefficients of thermal expansion (TEC) where the TEC of the holder is greater than or equal to the TEC of the sealing material. The TEC of the sealing material is in turn greater than or equal to the TEC of the fiber. It is preferred that the materials be selected so that their respective coefficients of thermal expansion are as close as possible to one another and they may all be equal. 4 figs.

Fiber optic assembly and method of making same

DOEpatents

Kramer, Daniel P.; Beckman, Thomas M.

1997-09-02

There is provided an assembly having a light guiding medium sealed to a her. Preferably the holder is a metal shell and a light guiding medium is an optical fiber of glass or sapphire whisker. The assembly includes a sealing medium which sealingly engages the metal holder to the fiber. In the formation of the assembly, the seal is essentially hermetic having a capability of minimizing leakage having a helium leak rate of less than 1.times.10.sup.-8 cubic centimeters per second and high strength having a capability of withstanding pressures of 100,000 psi or greater. The features of the assembly are obtained by a specific preparation method and by selection of specific starting materials. The fiber is selected to have a sufficiently high coefficient of thermal expansion which minimizes strains in the component during fabrication, as a result of fabrication, and during use. The other components are selected to be of a material having compatible coefficients of thermal expansion (TEC) where the TEC of the holder is greater than or equal to the TEC of the sealing material. The TEC of the sealing material is in turn greater than or equal to the TEC of the fiber. It is preferred that the materials be selected so that their respective coefficients of thermal expansion are as close as possible to one another and they may all be equal.

Air-soil exchange of organochlorine pesticides in a sealed chamber.

PubMed

Yang, Bing; Han, Baolu; Xue, Nandong; Zhou, Lingli; Li, Fasheng

2015-01-01

So far little is known about air-soil exchange under any sealed circumstances (e.g., in plastic and glass sheds), which however has huge implications for the soil-air-plant pathways of persistent organic pollutants including organochlorine pesticides (OCPs). A newly designed passive air sampler was tested in a sealed chamber for measuring the vertical concentration profiles of gaseous phase OCPs (hexachlorocyclohexanes (HCHs) and dichlorodiphenyltrichloroethanes (DDTs)). Air was sampled at 5, 15, and 30 cm above ground level every 10th day during a 60-day period by deploying polyurethane foam cylinders housed in acrylonitrile butadiene styrene-covered cartridges. Concentrations and compositions of OCPs along the vertical sections indicated a clear relationship with proximity to the mixture of HCHs and DDTs which escapes from the soils. In addition, significant positive correlations were found between air temperatures and concentrations of HCHs and DDTs. These results indicated revolatilization and re-deposition being at or close to dynamic pseudo-equilibrium with the overlying air. The sampler used for addressing air-soil exchange of persistent organic pollutants in any sealed conditions is discussed. Copyright © 2014. Published by Elsevier B.V.

Accelerated Lifetime Testing of Organic-Inorganic Perovskite Solar Cells Encapsulated by Polyisobutylene.

PubMed

Shi, Lei; Young, Trevor L; Kim, Jincheol; Sheng, Yun; Wang, Lei; Chen, Yifeng; Feng, Zhiqiang; Keevers, Mark J; Hao, Xiaojing; Verlinden, Pierre J; Green, Martin A; Ho-Baillie, Anita W Y

2017-08-02

Metal halide perovskite solar cells (PSCs) have undergone rapid progress. However, unstable performance caused by sensitivity to environmental moisture and high temperature is a major impediment to commercialization of PSCs. In the present work, a low-temperature, glass-glass encapsulation technique using high performance polyisobutylene (PIB) as the moisture barrier is investigated on planar glass/FTO/TiO 2 /FAPbI 3 /PTAA/gold perovskite solar cells. PIB was applied as either an edge seal or blanket layer. Electrical connections to the encapsulated PSCs were provided by either the FTO or Au layers. Results of a "calcium test" demonstrated that a PIB edge-seal effectively prevents moisture ingress. A shelf life test was performed and the PIB-sealed PSC was stable for at least 200 days. Damp heat and thermal cycling tests, in compliance with IEC61215:2016, were used to evaluate different encapsulation methods. Current-voltage measurements were performed regularly under simulated AM1.5G sunlight to monitor changes in PCE. The best results we have achieved to date maintained the initial efficiency after 540 h of damp heat testing and 200 thermal cycles. To the best of the authors' knowledge, these are among the best damp heat and thermal cycle test results for perovskite solar cells published to date. Given the modest performance of the cells (8% averaged from forward and reverse scans) especially with the more challenging FAPbI 3 perovskite material tested in this work, it is envisaged that better stability results can be further achieved when higher performance perovskite solar cells are encapsulated using the PIB packaging techniques developed in this work. We propose that heat rather than moisture was the main cause of our PSC degradation. Furthermore, we propose that preventing the escape of volatile decomposition products from the perovskite solar cell materials is the key for stability. PIB encapsulation is a very promising packaging solution for perovskite solar cells, given its demonstrated effectiveness, ease of application, low application temperature, and low cost.

Development of HgCdSe for Third Generation Focal Plane Arrays using Molecular Beam Epitaxy

DTIC Science & Technology

2013-08-01

quartz ampoules. Prior to the anneal, the quartz ampoules were etched in HF, pumped out to a vacuum of ~10 -5 Torr with a series of scroll and...and pumped down with a scroll pump to ≤10 -3 Torr. The load-lock was then switched from the scroll pump to a sorption pump cooled with liquid...focused on regions of (a) Ga 2p, (b) Sb 3d, (c) Sb 4d and Ga 3d, and (d) after annealing without atomic hydrogen (under vacuum ) at 400 °C for 30

Directional solidification of Pb-Sn eutectic with vibration

NASA Technical Reports Server (NTRS)

Caram, Rubens; Banan, Mohsen; Wilcox, William R.

1991-01-01

Pb-Sn eutectic alloy was directionally solidified at 1.4 to 3.2 cm/hr with forced convection induced by axial vibration of the growth ampoule with a frequency of 10 to 40 Hz and an amplitude of 0.5 to 1.0 mm. To determine the exact growth rate, an interface demarcation technique was applied. The lamellar spacing was increased 10 to 40 percent in ingots solidified with vibration compared to those solidified without vibration. The average intensity of convection in the melt under axial vibration of the ampoule was estimated by comparing the experimental results with a theoretical model.

Active Control of Interface Shape During the Crystal Growth of Lead Bromide

NASA Technical Reports Server (NTRS)

Duval, W. M. B.; Batur, C.; Singh, N. B.

2003-01-01

A thermal model for predicting and designing the furnace temperature profile was developed and used for the crystal growth of lead bromide. The model gives the ampoule temperature as a function of the furnace temperature, thermal conductivity, heat transfer coefficients, and ampoule dimensions as variable parameters. Crystal interface curvature was derived from the model and it was compared with the predicted curvature for a particular furnace temperature and growth parameters. Large crystals of lead bromide were grown and it was observed that interface shape was in agreement with the shape predicted by this model.

Reduction-oxidation Enabled Glass-ceramics to Stainless Steel Bonding Part I: screening of doping oxidants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dai, Steve Xunhu

Lithium silicate-based glass-ceramics with high coefficients of thermal expansion, designed to form matched hermetic seals in 304L stainless steel housing, show little evidence of interfacial chemical bonding, despite extensive inter-diffusion at the glass-ceramic-stainless steel (GC-SS) interface. A series of glass-ceramic compositions modified with a variety of oxidants, AgO, FeO, NiO, PbO, SnO, CuO, CoO, MoO 3 and WO 3, are examined for the feasibility of forming bonding oxides through reduction-oxidation (redox) at the GC-SS interface. The oxidants were selected according to their Gibbs free energy to allow for oxidation of Cr/Mn/Si from stainless steel, and yet to prevent a reductionmore » of P2O5 in the glass-ceramic where the P 2O 5 is to form Li 3PO 4 nuclei for growth of high expansion crystalline SiO 2 phases. Other than the CuO and CoO modified glass-ceramics, bonding from interfacial redox reactions were not achieved in the modified glass-ceramics, either because of poor wetting on the stainless steel or a reduction of the oxidants at the surface of glass-ceramic specimens rather than the GC-SS interface.« less

Rhenium solubility in borosilicate nuclear waste glass: implications for the processing and immobilization of technetium-99.

PubMed

McCloy, John S; Riley, Brian J; Goel, Ashutosh; Liezers, Martin; Schweiger, Michael J; Rodriguez, Carmen P; Hrma, Pavel; Kim, Dong-Sang; Lukens, Wayne W; Kruger, Albert A

2012-11-20

The immobilization of technetium-99 ((99)Tc) in a suitable host matrix has proven to be a challenging task for researchers in the nuclear waste community around the world. In this context, the present work reports on the solubility and retention of rhenium, a nonradioactive surrogate for (99)Tc, in a sodium borosilicate glass. Glasses containing target Re concentrations from 0 to 10,000 ppm [by mass, added as KReO(4) (Re(7+))] were synthesized in vacuum-sealed quartz ampules to minimize the loss of Re from volatilization during melting at 1000 °C. The rhenium was found as Re(7+) in all of the glasses as observed by X-ray absorption near-edge structure. The solubility of Re in borosilicate glasses was determined to be ~3000 ppm (by mass) using inductively coupled plasma optical emission spectroscopy. At higher rhenium concentrations, additional rhenium was retained in the glasses as crystalline inclusions of alkali perrhenates detected with X-ray diffraction. Since (99)Tc concentrations in a glass waste form are predicted to be <10 ppm (by mass), these Re results implied that the solubility should not be a limiting factor in processing radioactive wastes, assuming Tc as Tc(7+) and similarities between Re(7+) and Tc(7+) behavior in this glass system.

Surface sealing using self-assembled monolayers and its effect on metal diffusion in porous low-k dielectrics studied using monoenergetic positron beams

NASA Astrophysics Data System (ADS)

Uedono, Akira; Armini, Silvia; Zhang, Yu; Kakizaki, Takeaki; Krause-Rehberg, Reinhard; Anwand, Wolfgang; Wagner, Andreas

2016-04-01

Surface sealing effects on the diffusion of metal atoms in porous organosilicate glass (OSG) films were studied by monoenergetic positron beams. For a Cu(5 nm)/MnN(3 nm)/OSG(130 nm) sample fabricated with pore stuffing, C4F8 plasma etch, unstuffing, and a self-assembled monolayer (SAM) sealing process, it was found that pores with cubic pore side lengths of 1.1 and 3.1 nm coexisted in the OSG film. For the sample without the SAM sealing process, metal (Cu and Mn) atoms diffused from the top Cu/MnN layer into the OSG film and were trapped by the pores. As a result, almost all pore interiors were covered with those metals. For the sample damaged by an Ar/C4F8 plasma etch treatment before the SAM sealing process, SAMs diffused into the OSG film, and they were preferentially trapped by larger pores. The cubic pore side length in these pores containing self-assembled molecules was estimated to be 0.7 nm. Through this work, we have demonstrated that monoenergetic positron beams are a powerful tool for characterizing capped porous films and the trapping of atoms and molecules by pores.

EFFECTS OF ONE WEEK TRITIUM EXPOSURE ON EPDM ELASTOMER

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, E

This report documents test results for the exposure of four formulations of EPDM (ethylene-propylene diene monomer) elastomer to tritium gas at one atmosphere for approximately one week and characterization of material property changes and changes to the exposure gas during exposure. All EPDM samples were provided by Los Alamos National Laboratory (LANL). Material properties that were characterized include mass, sample dimensions, appearance, flexibility, and dynamic mechanical properties. The glass transition temperature was determined by analysis of the dynamic mechanical property data per ASTM standards. No change of glass transition temperature due to the short tritium gas exposure was observed. Filledmore » and unfilled formulations of Dupont{reg_sign} Nordel{trademark} 1440 had a slightly higher glass transition temperature than filled and unfilled formulations of Uniroyal{reg_sign} Royalene{reg_sign} 580H; filled formulations had the same glass transition as unfilled. The exposed samples appeared the same as before exposure--there was no evidence of discoloration, and no residue on stainless steel spacers contacting the samples during exposure was observed. The exposed samples remained flexible--all formulations passed a break test without failing. The unique properties of polymers make them ideal for certain components in gas handling systems. Specifically, the resiliency of elastomers is ideal for sealing surfaces, for example in valves. EPDM, initially developed in the 1960s, is a hydrocarbon polymer used extensively for sealing applications. EPDM is used for its excellent combination of properties including high/low-temperature resistance, radiation resistance, aging resistance, and good mechanical properties. This report summarizes initial work to characterize effects of tritium gas exposure on samples of four types of EPDM elastomer: graphite filled and unfilled formulations of Nordel{trademark} 1440 and Royalene{reg_sign} 580H.« less

In vitro mechanical stimulation facilitates stress dissipation and sealing ability at the conventional glass ionomer cement-dentin interface.

PubMed

Toledano, Manuel; Osorio, Raquel; Osorio, Estrella; Cabello, Inmaculada; Toledano-Osorio, Manuel; Aguilera, Fátima S

2018-06-01

The aim of this study was to evaluate the induced changes in the chemical and mechanical performance at the glass-ionomer cement-dentin interface after mechanical load application. A conventional glass-ionomer cement (GIC) (Ketac Bond), and a resin-modified glass-ionomer cement (RMGIC) (Vitrebond Plus) were used. Bonded interfaces were stored in simulated body fluid, and then tested or submitted to the mechanical loading challenge. Different loading waveforms were applied: No cycling, 24 h cycled in sine or loaded in sustained hold waveforms. The cement-dentin interface was evaluated using a nano-dynamic mechanical analysis, estimating the complex modulus and tan δ. Atomic Force Microscopy (AFM) imaging, Raman analysis and dye assisted confocal microscopy evaluation (CLSM) were also performed. The complex modulus was lower and tan delta was higher at interfaces promoted with the GIC if compared to the RMGIC unloaded. The conventional GIC attained evident reduction of nanoleakage. Mechanical loading favored remineralization and promoted higher complex modulus and lower tan delta values at interfaces with RMGIC, where porosity, micropermeability and nanoleakage were more abundant. Mechanical stimuli diminished the resistance to deformation and increased the stored energy at the GIC-dentin interface. The conventional GIC induced less porosity and nanoleakage than RMGIC. The RMGIC increased nanoleakage at the porous interface, and dye sorption appeared within the cement. Both cements created amorphous and crystalline apatites at the interface depending on the type of mechanical loading. Remineralization, lower stress concentration and resistance to deformation after mechanical loading improved the sealing of the GIC-dentin interface. In vitro oral function will favor high levels of accumulated energy and permits micropermeability at the RMGIC-dentin interface which will become remineralized. Copyright © 2018 Elsevier Ltd. All rights reserved.

Silicone-Rubber Microvalves Actuated by Paraffin

NASA Technical Reports Server (NTRS)

Svelha, Danielle; Feldman, Sabrina; Barsic, David

2004-01-01

Microvalves containing silicone-rubber seals actuated by heating and cooling of paraffin have been proposed for development as integral components of microfluidic systems. In comparison with other microvalves actuated by various means (electrostatic, electromagnetic, piezoelectric, pneumatic, and others), the proposed valves (1) would contain simpler structures that could be fabricated at lower cost and (2) could be actuated by simpler (and thus less expensive) control systems. Each valve according to the proposal would include a flow channel bounded on one side by a flat surface and on the other side by a curved surface defined by an arched-cross-section, elastic seal made of silicone rubber [polydimethylsilane (PDMS)]. The seal would be sized and shaped so that the elasticity of the PDMS would hold the channel open except when the seal was pressed down onto the flat surface to close the channel. The principle of actuation would exploit the fact that upon melting or freezing, the volume of a typical paraffin increases or decreases, respectively, by about 15 percent. In a valve according to the proposal, the seal face opposite that of the channel would be in contact with a piston-like plug of paraffin. In the case of a valve designed to be normally open at ambient temperature, one would use a paraffin having a melting temperature above ambient. The seal would be pushed against the flat surface to close the channel by heating the paraffin above its melting temperature. In the case of a valve designed to be normally closed at ambient temperature, one would use a paraffin having a melting temperature below ambient. The seal would be allowed to spring away from the flat surface to open the channel by cooling the paraffin below its melting temperature. The availability of paraffins that have melting temperatures from 70 to +80 C should make it possible to develop a variety of normally closed and normally open valves. The figure depicts examples of prototype normally open and normally closed valves according to the proposal. In each valve, an arch cross section defining a channel having dimensions of the order of tens of micrometers would be formed in a silicone-rubber sheet about 40 m thick. The silicone rubber sheet would be hermetically sealed to a lower glass plate that would define the sealing surface and to an upper glass plate containing a well. The well would be filled with paraffin and capped with a rigid restraining layer of epoxy. In the normally open valve, the paraffin would have a melting temperature above ambient (e.g., 40 C) and the wall of the well would be coated with a layer of titanium that would serve as an electric heater. In the normally closed valve, the paraffin would have a melting temperature below ambient (e.g.-5 C). Instead of a heater in the well, the normally closed valve would include a thermoelectric cooler on top of the epoxy cap.

Synthesis, characterization and processing of active rare earth-doped chalcohalide glasses

NASA Astrophysics Data System (ADS)

Debari, Roberto Mauro

Applications for infrared-transmitting non-oxide glass fibers span a broad range of topics. They can be used in the military, the medical field, telecommunications, and even in agriculture. Rare earth ions are used as dopants in these glasses in order to stimulate emissions in the infrared spectral region. In order to extend the host glass transmission further into the infrared, selenium atoms were substituted for sulfur in the established Ge-S-I chalcohalide glass system and the fundamental properties of these latter glasses were explored. Over 30 different compositions in the Ge-Se-I glass system were investigated as to their thermal and optical properties. The resulting optimum host with a composition of Ge15Se80I5 has a broad transmission range from 0.7 mum to 17.0 mum and a high working range over 145°C. The host glass also exhibited a Tg of 125°C, making rotational casting of a cladding tube for rod-and-tube fiberization a possibility. The base glass was doped with 1000 to 4000 ppm/wt of erbium, dysprosium, or neodymium. When doped with Er3+-ions, absorptions at 1.54 mum and 3.42 mum were observed. Nd3+-doping resulted in an absorption peak near 4.24 mum and Dy3+ ions caused absorption at 1.30 mum. Fluorescence emissions were found for neodymium at 1.396 mum with a FWHM of 74 nm, and for dysprosium at 1.145 mum with a FWHM of 75 nm, at 1.360 mum with a FWHM of 98 rim and at 1.674 mum with a FWHM of 60 nm. High optical quality tubes of the host glass could be formed using rotational casting in silica ampoules. Glass tubes, 4 to 6 cm long with a 1 cm outer diameter and a tailored inner-hole diameter ranging from 0.4 to 0.6 cm could be synthesized by this process with excellent dimensional tolerances around the circumference as well as along the length. A preform of this size provided 25 continuous meters of unclad fiber with diameters ranging from 140 to 200 mum. A UV-curable acrylate cladding was applied via an external coating cup. An x-ray analysis of the resulting fiber verified the constituents of the fiber. Due to tradeoffs between thermal properties, optical properties and rare earth solubility, the Ge-Se-I glass system must still be optimized prior to use as an active fiber device. Nevertheless, the viability of this host system has been demonstrated in this investigation. Some very promising advantages to adding halides to chalcogenide glass systems have been confirmed, including the tailoring of glass transition temperatures, enhancement of rare earth solubility, expanded fluorescence emissions in the IR, and suppression of some impurity absorption bands. Also, the potential for rod-and-tube fiberization utilizing the rotational casting method for tube synthesis has been established along with its resulting pristine core-clad interface. This research provides a foundation for active fiber device applications in the 2 to 10 mum spectral region.

Apollo 14 crewmembers sealed inside a Mobile Quarantine Facility

NASA Technical Reports Server (NTRS)

1971-01-01

Separated by aluminum and glass of their Mobile Quarantine Facility (MQF), the Apollo 14 crewmen visit with their families and friends upon arriving at Ellington Air Force Base in the early morning hours of February 12, 1971. Looking through the MQF window are Astronats Alan B Shepard Jr. (left); Stuart A Roosa (right); and Edgar D. Mitchell.

The "Magical" Sphere: Uncovering the Secret

ERIC Educational Resources Information Center

Petruševski, Vladimir M.; Bukleski, Miha

2006-01-01

A red sphere is seen at the bottom of a sealed glass tube filled with a colorless, transparent liquid. Holding the tube for a short period makes the sphere rise slowly from the bottom until it finally floats on the surface of the liquid. Instructions for preparing the demonstration are given, together with an explanation of the phenomenon. A…

Void Management in MEPHISTO and Other Space Experiments

NASA Technical Reports Server (NTRS)

deGroh, Henry C., III; Johnston, J. Christopher; Wei, Bingbo

1998-01-01

The second flight of NASA's Shuttle Flight experiment program known as MEPHISTO suffered from a void in the liquid portion of the sample, even though a piston arrangement was in place to keep the ampoule filled. In preparations for the next flight of the MEPHISTO furnace an animated computer program, called MEPHISTO Volume Visualizer (MVV), was written to help avoid the formation of unwanted voids. A piston system on MEPHISTO has the ability to move approximately 5 mm in compression, to accommodate expansion of the solid during heating; then from the completely compressed position, the piston can move up to 25 mm in towards the sample, effectively making the ampoule smaller and hopefully eliminating any voids. Due to the nature of the piston design and ampoule and sample arrangement, the piston has gotten stuck during normal directional solidification; this creates the risk of a void. To eliminate such a void, the liquid in the hot zones of the furnace can be heated, thereby expanding the liquid and consuming any void. The problem with this approach is that if the liquid is heated too much an overpressure could result, breaking the ampoule and ending the experiment catastrophically. The MVV has been found to be a useful tool in the assessment of the risks associated with the formation of a void and the additional heating of the liquid in the hot zone of this Bridgman type furnace. The MVV software will be discussed and copies available; it is written in the Delphi 2 programming language and runs under Windows 95 and NT. The strategies used in other flight experiments, such as the Isothermal Dendritic Growth Experiment, will also be presented.

Prescribing injectable and oral methadone to opiate addicts: results from the 1995 national postal survey of community pharmacies in England and Wales.

PubMed Central

Strang, J.; Sheridan, J.; Barber, N.

1996-01-01

OBJECTIVE--To establish the extent of prescribing injectable and oral methadone to opiate addicts and the practice characteristics and dispensing arrangements attached to these prescriptions. DESIGN--National survey of 25% random sample of community (high street) pharmacies through postal questionnaire, with four mailings. SETTING--England and Wales. SUBJECTS--1 in 4 sample of all 10,616 community pharmacies, stratified by family health services authority. MAIN OUTCOME MEASURES--Data were collected on each prescription for controlled drugs currently being dispensed by pharmacies to misusers, describing the drug, form, dose, source (general practice or hospital; and NHS or private), and numbers of dispensing pick ups a week. RESULTS--Methadone was the opiate most commonly dispensed to misusers (96.0% of 3846 opiate prescriptions). 79.6% of methadone prescriptions were for the oral liquid form, 11.0% for tablet, and 9.3% for injectable ampoules. More than one third of all methadone prescriptions were for weekly or fortnightly pick up, with a further third being for daily pick up. Tablets and ampoules were even less likely to be dispensed on a daily basis. Private prescriptions were significantly more likely than NHS ones to be for tablets or ampoules, to be for substantially higher daily doses, and to be collected on a weekly or fortnightly basis. CONCLUSIONS--The distinctively British practice of prescribing injectable methadone was found to be widespread and, contrary to guidance, to be as prevalent in non-specialist as specialist settings. In view of the frequent crushing and injecting of methadone tablets, clearer more authoritative guidance is needed on the contexts in which injectable methadone (tablets as well as ampoules) should be prescribed and on the responsibilities for monitoring and supervision which should be attached. PMID:8704540

Accessibility and potency of uterotonic drugs purchased by simulated clients in four districts in India.

PubMed

Stanton, Cynthia; Nand, Deepak Nitya; Koski, Alissa; Mirzabagi, Ellie; Brooke, Steve; Grady, Breanne; Mullany, Luke C

2014-11-13

Surveillance of drug quality for antibiotics, antiretrovirals, antimalarials and vaccines is better established than surveillance for maternal health drugs in low-income countries, particularly uterotonic drugs for the prevention and treatment of postpartum hemorrhage. The objectives of this study are to: assess private sector accessibility of four drugs used for uterotonic purposes (oxytocin, methylergometrine, misoprostol, valethamate bromide); and to assess potency of oxytocin and methylergometrine ampoules purchased by simulated clients. The study was conducted in Hassan and Bagalkot districts in Karnataka state and Agra and Gorakhpur districts in Uttar Pradesh state. A sample of 877 private pharmacies was selected (using a stratified, systematic sampling with random start), among which 847 were successfully visited. The target sample size for assessment of accessibility was 50 pharmacies per drug, per district. The target sample size for potency assessment was 100 purchases each of oxytocin and methylergometrine across all districts. Successful drug purchases varied by state. In Agra and Gorakhpur, 90%-100% of visits for each of the drugs resulted in a purchase. In Bagalkot and Hassan, only 29%-52% of visits for each drug resulted in a purchase. Regarding potency, the percent of active pharmaceutical ingredient was assessed using United States Pharmacopeia monograph #33 for both drugs; 193 and 188 ampoules of oxytocin and methylergometrine, respectively, were assessed. The percent of oxytocin ampoules outside manufacturer specification ranged from 33%-40% in Karnataka and from 22%-50% in Uttar Pradesh. In Bagalkot and Hassan, 96% and 100% of the methylergometrine ampoules were outside manufacturer specification, respectively. In Agra and Gorakhpur, 54% and 44% were outside manufacturer specification, respectively. Private sector accessibility of uterotonic drugs in study districts in Karnataka warrants attention. Most importantly, interventions to assure quality oxytocin and particularly methylergometrine are needed in study districts in both states.

Development of a high temperature ceramic-to-metal seal for Air Force Weapons Laboratory Laser

NASA Astrophysics Data System (ADS)

Honnell, R. E.; Stoddard, S. D.

1987-03-01

Procedures were developed for fabricating vacuum tight metal-to-ceramic ring seals between Inconel 625 and MgO-3 wt % Y2O3 tubes metallized with a calcia-alumina-silica glass (CaO-29 wt % Al2O3-35 wt % SiO2) containing 50 vol % molybdenum filler. Palniro No. 1 (Au-25 wt % Pd-25 wt % Ni) was found to be the most reliable braze for joining Inconel to metallized MgO-3 wt % Y2O3 bodies. The reliabilities of the processing procedures and the material systems were demonstrated. A prototype electrical feedthrough was fabricated for 1173 K operation in air or vacuum.

Liquid hyperpolarized 129Xe produced by phase exchange in a convection cell

NASA Astrophysics Data System (ADS)

Su, T.; Samuelson, G. L.; Morgan, S. W.; Laicher, G.; Saam, B.

2004-09-01

We present a method for the production of liquid hyperpolarized Xe129 that employs spin-exchange optical pumping in the gas phase and subsequent phase exchange with a column of xenon liquid. A convection loop inside the sealed glass cell allows efficient transfer of magnetization between the gas and liquid phases. By condensing to liquid a large fraction of the sample, this scheme permits the polarization of many more Xe129 atoms in a given sealed-cell volume than would otherwise be possible. We have thus far produced a steady-state polarization of 8% in 0.1mL of liquid with a characteristic rise time of ≈15min.

Fast production of microfluidic devices by CO2 laser engraving of wax-coated glass slides.

PubMed

da Costa, Eric T; Santos, Mauro S F; Jiao, Hong; do Lago, Claudimir L; Gutz, Ivano G R; Garcia, Carlos D

2016-07-01

Glass is one of the most convenient materials for the development of microfluidic devices. However, most fabrication protocols require long processing times and expensive facilities. As a convenient alternative, polymeric materials have been extensively used due their lower cost and versatility. Although CO2 laser ablation has been used for fast prototyping on polymeric materials, it cannot be applied to glass devices because the local heating causes thermal stress and results in extensive cracking. A few papers have shown the ablation of channels or thin holes (used as reservoirs) on glass but the process is still far away from yielding functional glass microfluidic devices. To address these shortcomings, this communication describes a simple method to engrave glass-based capillary electrophoresis devices using standard (1 mm-thick) microscope glass slides. The process uses a sacrificial layer of wax as heat sink and enables the development of both channels (with semicircular shape) and pass-through reservoirs. Although microscope images showed some small cracks around the channels (that became irrelevant after sealing the engraved glass layer to PDMS) the proposed strategy is a leap forward in the application of the technology to glass. In order to demonstrate the capabilities of the approach, the separation of dopamine, catechol and uric acid was accomplished in less than 100 s. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of Gd2O3 doping on structure and boron volatility of borosilicate glass sealants in solid oxide fuel cells-A study on the La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode

NASA Astrophysics Data System (ADS)

Zhang, Qi; Tan, Shengwei; Ren, Mengyuan; Yang, Hsiwen; Tang, Dian; Chen, Kongfa; Zhang, Teng; Jiang, San Ping

2018-04-01

Boron volatility is one of the most important properties of borosilicate-based glass sealants in solid oxide fuel cells (SOFCs), as boron contaminants react with lanthanum-containing cathodes, forming LaBO3 and degrading the activity of SOFCs. Here, we report that the reaction between the volatile boron and a La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode during polarization can be significantly reduced by doping aluminoborosilicate glass with Gd2O3. Specifically, the Gd cations in glass with 2 mol.% Gd2O3 dissolve preferentially in the borate-rich environment to form more Gd-metaborate structures and promote the formation of calcium metaborate (CaB2O4); they also condense the B-O network after heat treatment, which suppresses poisoning by boron contaminants on the LSCF cathode. The results provide insights into design and development of a reliable sealing glass for SOFC applications.

Hermetic aluminum radio frequency interconnection and method for making

DOEpatents

Kilgo, Riley D.; Kovacic, Larry; Brow, Richard K.

2000-01-01

The present invention provides a light-weight, hermetic coaxial radio-frequency (RF) interconnection having an electrically conductive outer housing made of aluminum or an aluminum alloy, a central electrical conductor made of ferrous or non-ferrous material, and a cylinder of dielectric material comprising a low-melting-temperature, high-thermal-expansion aluminophosphate glass composition for hermetically sealing between the aluminum-alloy outer housing and the ferrous or non-ferrous center conductor. The entire RF interconnection assembly is made permanently hermetic by thermally fusing the center conductor, glass, and housing concurrently by bringing the glass to the melt point by way of exposure to an atmospheric temperature sufficient to melt the glass, less than 540.degree. C., but that does not melt the center conductor or the outer aluminum or aluminum alloy housing. The composition of the glass used is controlled to provide a suitable low dielectric constant so that an appropriate electrical characteristic impedance, for example 50 ohms, can be achieved for an electrical interconnection that performs well at high radio frequencies and also provides an interconnection maintaining a relatively small physical size.

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

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Gamble, Eleanor A.

2005-01-01

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.

Multi-pane glass unit having seal with adhesive and hermetic coating layer

DOEpatents

Miller, Seth A; Stark, David H; Francis, IV, William H; Puligandla, Viswanadham; Boulos, Edward N; Pernicka, John

2015-02-10

A vacuum insulated glass unit (VIGU) comprises a first pane of a transparent material and a second pane of a transparent material. The second pane is spaced apart from the first pane to define a cavity therebetween. At least one of a spacer and an array of stand-off members is disposed between the first and second panes to maintain separation therebetween. A first adhesive layer forms at least a portion of a gas-tight connection between the first pane and the second pane. A highly hermetic coating is disposed over the adhesive layer, where the coating is an inorganic layer.

Modular packaging concept for MEMS and MOEMS

NASA Astrophysics Data System (ADS)

Stenchly, Vanessa; Reinert, Wolfgang; Quenzer, Hans-Joachim

2017-11-01

Wherever technical systems detect objects in their environment or interact with people, optical devices may play an important role. Light can be relatively easily produced and spatially and temporally modulated. Laser can project sharp images over long distances or cut materials in short distances. Depending on the wavelength an invisible scanning in near infrared for gesture recognition is possible as well as a projection of brilliant colour images. For several years, the Fraunhofer ISIT develops Opto-Packaging processes based on the viscous reshaping of glass wafers: First, hermetically sealed laser micro-mirror scanners WLP with inclined windows deflect in the central light reflex of the window out of the image area. Second, housing with lateral light exit permits hermetic sealing of edge-emitting lasers for highest reliability and durability. Such systems are currently experiencing an extremely high interest of the industry in all segments, from consumer to automotive through to materials processing. Our modular Opto-Packaging platform enables fast product developments. Housing for opto mechanical MEMS devices are equipped with inclined windows to minimize distortion, stray light and reflection losses. The hot viscous glass forming technology is also applied to functionalized substrate wafers which possess areas with high heat dissipation in addition to thermally insulating areas. Electrical contacts may be realized with metal filled vias or TGV (Through Glass Vias). The modular system reduces the development times for new, miniaturized optical systems so that manufacturers can focus on the essentials in their development, namely their product functionalities.

Collection-efficient, axisymmetric vacuum sublimation module for the purification of solid materials.

PubMed

May, Michael; Paul, Elizabeth; Katovic, Vladimir

2015-11-01

A vacuum sublimation module of axisymmetric geometry was developed and employed to purify solid-phase materials. The module provides certain practical advantages and it comprises: a metering valve, glass collector, glass lower body, main seal, threaded bushing, and glass internal cartridge (the latter to contain starting material). A complementary process was developed to de-solvate, sublime, weigh, and collect solid chemical materials exemplified by oxalic acid, ferrocene, pentachlorobenzene, chrysene, and urea. The oxalic acid sublimate was analyzed by titration, melting range, Fourier Transform Infrared (FT-IR) Spectroscopy, cyclic voltammetry, and its (aqueous phase) electrolytically generated gas. The analytical data were consistent with a high-purity, anhydrous oxalic acid sublimate. Cyclic voltammograms of 0.11 mol. % oxalic acid in water displayed a 2.1 V window on glassy carbon electrode beyond which electrolytic decomposition occurs. During module testing, fifteen relatively pure materials were sublimed with (energy efficient) passive cooling and the solid-phase recovery averaged 95 mass %. Key module design features include: compact vertical geometry, low-angle conical collector, uniformly compressed main seal, modest power consumption, transparency, glovebox compatibility, cooling options, and preferential conductive heat transfer. To help evaluate the structural (module) heat transfer, vertical temperature profiles along the dynamically evacuated lower body were measured versus electric heater power: for example, an input of 18.6 W generated a temperature 443-K at the bottom. Experimental results and engineering calculations indicate that during sublimation, solid conduction is the primary mode of heat transfer to the starting material.

Directional solidification of Pb-Sn eutectics with vibration

NASA Technical Reports Server (NTRS)

Caram, Rubens; Banan, Mohsen; Wilcox, William R.

1991-01-01

Pb-Sn eutectic alloy was directionally solidified at 1.4 to 3.2 cm/hr with forced convection induced by axial vibration of the growth ampoule with a frequency of 10 to 40 Hz and an amplitude of 0.5 to 1.0 mm. To determine the exact growth rate, an interface demarcation technique was applied. The lamellar spacing was increased 10 to 40 percent in ingots solidified with vibration compared to those solidified without vibration. The number of grain boundaries was increased by vibration. The average intensity of convection in the melt under axial vibration of the ampoule was estimated by comparing the experimental results with a theoretical model.

Preparation of superhydrophobic and transparent micro-nano hybrid coatings from polymethylhydroxysiloxane and silica ormosil aerogels

NASA Astrophysics Data System (ADS)

Nagappan, Saravanan; Park, Jin Joo; Park, Sung Soo; Ha, Chang-Sik

2014-12-01

Superhydrophobic and transparent polymethylhydroxysiloxane (PMHOS)/silica ormosil aerogel hybrids were prepared successfully by mixing of PMHOS with various weight percentages of silica ormosil aerogels (as synthesized from methyltriethoxysilane (MTES) and methyltrimethoxysilane (MTMS) precursors) in separate seal perfume glass vials. The hybrids were spin coated on glass substrate at 1000 rpm for 60 seconds and used for further analysis. The surface morphology and chemical compositions of the hybrids were analyzed by high resolution scanning electron microscopy, high resolution transmission electron microscopy, atomic force spectroscopy, adsorption and desorption isotherm, and X-ray photoelectron spectroscopy. The transparency, thermal decomposition and static contact angle (SCA) of each sample were measured by UV-Visible spectrophotometer, TGA and drop shape analysis system, respectively. The spin coated substrates showed good superhydrophobic properties, thermal stability as well as transparency on the glass substrates.

Mechanochemically synthesized kalsilite based bioactive glass-ceramic composite for dental vaneering

NASA Astrophysics Data System (ADS)

Kumar, Pattem Hemanth; Singh, Vinay Kumar; Kumar, Pradeep

2017-08-01

Kalsilite glass-ceramic composites have been prepared by a mechanochemical synthesis process for dental veneering application. The aim of the present study is to prepare bioactive kalsilite composite material for application in tissue attachment and sealing of the marginal gap between fixed prosthesis and tooth. Mechanochemical synthesis is used for the preparation of microfine kalsilite glass-ceramic. Low temperature frit and bioglass have been prepared using the traditional quench method. Thermal, microstructural and bioactive properties of the composite material have been examined. The feasibility of the kalsilite to be coated on the base commercial opaque as well as the bioactive behavior of the coated specimen has been confirmed. This study indicates that the prepared kalsilite-based composites show similar structural, morphological and bioactive behavior to that of commercial VITA VMK95 Dentin 1M2.

Wood liquefaction and its application to Novolac resin

Treesearch

Hui Pan; Chung-Yun Hse; Todd F. Shupe

2009-01-01

Wood liquefaction was conducted using phenol as a reagent solvent with a weak acid catalyst in two different reactors: (Alma et al., 1995a.) an atmospheric glass reactor and (Alma et al., 1995b.) a sealed Parr® reactor. Residues were characterized by wet chemical analyses, Fourier transform infrared (FT-IR) spectroscopy, and X-ray diffraction (XRD). The FT-IR...

Needlestick and Sharps Injuries Among Nursing Students in Nanjing, China.

PubMed

Zhang, Xujun; Chen, Yu; Li, Yang; Hu, Jie; Zhang, Cong; Li, Zhen; Stallones, Lorann; Xiang, Henry

2018-06-01

Needlestick and sharps injuries (NSIs) are a major cause of occupational injuries for health care workers worldwide. In this study, the authors report the prevalence of and risk factors for NSIs among Chinese nursing students. A cross-sectional survey was distributed to 442 nursing students; 393 completed questionnaires were submitted. A total of 237 (60.3%) nursing students reported NSIs, which were more commonly reported by female students, younger students, students who worked frequent night shifts, students without safety training, and students who did not use personal protective equipment. Among those injured, 59.9% were injured by syringe needles, 21.9% by glass items, and 3.4% by scissors. Of those needles and sharps causing injuries, 36.3% of devices had been used on patients, 41% were unused, and 22.7% were unknown. Opening ampoules or vials was the most common injury agent. A total of 86.9% of NSIs were not reported to hospital infection control. Nursing students are at high risk of NSIs in China. Occupational safety training should be developed and implemented to prevent NSIs among this vulnerable population.

A morphological study of the sulfurisation of digenite to covellite using reflected polarised light microscopy

NASA Astrophysics Data System (ADS)

Rask Møller Frøkiær, Heidi; Warner, Terence E.

2017-08-01

A series of copper rods were reacted with sulfur vapour in evacuated glass ampoules at ∼445 °C. Product materials were characterised by powder X-ray diffraction and reflected polarised light microscopy. Copper sulfurised rapidly to digenite, γ-Cu2-xS, under these conditions, whereas the subsequent sulfurisation to covellite, CuS, was notably slower, yielding texturally distinguishable inner (secondary) and outer (primary) CuS regions. A two-stage partial sulfurisation of γ-Cu1.8S resulted in the external growth of two successive layers of primary CuS, which demonstrates decisively that covellite - besides being a p-type metal - is ionically conducting at 445 °C, although considerably less so than digenite. We infer that the growth of platy covellite crystals and their radial alignment in the primary CuS layer are a consequence of copper ion mobility being restricted to the basal plane of the covellite structure. Sulfurising a coil of copper wire at ∼445 °C is an effective method for synthesising covellite.

Chemical dosimetry system for criticality accidents.

PubMed

Miljanić, Saveta; Ilijas, Boris

2004-01-01

Ruder Bosković Institute (RBI) criticality dosimetry system consists of a chemical dosimetry system for measuring the total (neutron + gamma) dose, and a thermoluminescent (TL) dosimetry system for a separate determination of the gamma ray component. The use of the chemical dosemeter solution chlorobenzene-ethanol-trimethylpentane (CET) is based on the radiolytic formation of hydrochloric acid, which protonates a pH indicator, thymolsulphonphthalein. The high molar absorptivity of its red form at 552 nm is responsible for a high sensitivity of the system: doses in the range 0.2-15 Gy can be measured. The dosemeter has been designed as a glass ampoule filled with the CET solution and inserted into a pen-shaped plastic holder. For dose determinations, a newly constructed optoelectronic reader has been used. The RBI team took part in the International Intercomparison of Criticality Accident Dosimetry Systems at the SILENE Reactor, Valduc, June 2002, with the CET dosimetry system. For gamma ray dose determination TLD-700 TL detectors were used. The results obtained with CET dosemeter show very good agreement with the reference values.

Vacuum-sealed microcavity formed from suspended graphene by using a low-pressure dry-transfer technique

NASA Astrophysics Data System (ADS)

Takahashi, K.; Ishida, H.; Sawada, K.

2018-01-01

We report the development of a microcavity drum sealed by suspended graphene. The drum is fabricated by using a low-pressure dry-transfer technique, which involves vacuum de-aeration between a graphene sheet and a substrate and raising the temperature to above the glass transition of the supporting poly(methyl methacrylate) film, which serves to increase the real contact area. The result is a suspended graphene sheet with a maximum diameter of 48.6 μm. The Raman spectrum of the suspended graphene has a 2D/G ratio of 1.79 and a few D peaks, which suggests that the material is high-quality single-layer graphene. The dry-transfer technique yields a vacuum-sealed microcavity drum 1.1 μm deep up to 4.5 μm in diameter. The Raman shift indicates that the suspended graphene is subjected to a tensile strain of 0.05%, which is attributed to the pressure difference between the evacuated cavity and the exterior gas.

Durability of symmetric-structured metal-supported solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Tucker, Michael C.

2017-11-01

Symmetric-structure metal-supported solid oxide fuel cells (MS-SOFC) with YSZ electrolyte are fabricated with porous YSZ backbone electrodes, stainless steel supports, and infiltrated catalysts on both anode and cathode side. Durability towards aggressive thermal and redox cycling, and long-term operation is assessed. Many sealing material candidates are screened for compatibility with the cell materials and operating conditions, and a commercial sealing glass, GM31107, is selected. LSM/SDCN cells are then subjected to 200 very fast thermal cycles and 20 complete redox cycles, with minimal impact to cell performance. LSM/SDCN and SDCN/SDCN cells are operated for more than 1200 h at 700 °C. The seal and cell hermeticity is maintained, and cell ohmic impedance does not change significantly during operation. Electrode polarization increases during operation, leading to significant degradation of the cell performance. In-operando EIS and post-mortem SEM/EDS analysis suggest that catalyst coarsening and cathode Cr deposition are the dominant degradation modes.

A comparative evaluation of sealing ability of four root end filling materials using fluid filtration method: An in vitro study

PubMed Central

Shetty, Shilpa; Hiremath, Geeta; Yeli, Mahantesh

2017-01-01

Aim of the Study: The aim of this study was to compare and evaluate the sealing ability of four root end filling materials mineral trioxide aggregate (MTA)-Plus, Biodentine, MTA (MTA Angelus) and glass ionomer cement (GIC) using fluid filtration method. Materials and Methods: Forty-four extracted, human single-rooted teeth were collected. The crown of each tooth was decoronated 2 mm above the cementoenamel junction. Canals were negotiated, instrumented, obturated using lateral compaction method. The access cavities were sealed with Cavit. Root end resection and apical root end cavity preparations of 4 mm were made in each specimen. The selected roots were then randomly divided into four groups (n = 11) and restored as follows. Group 1 – GIC, Group 2 – MTA (MTA Angelus), Group 3 – Biodentine, and Group 4 – MTA Plus. The apical microleakage of each specimen was assessed using fluid filtration method at 72 h, 1 month and 3 months. Microleakage in each specimen was recorded in mm (millimeter) and converted to μl/min/cm H2O. Results: MTA Angelus showed least microleakage followed by Biodentine and MTA Plus. Least sealing ability was seen with GIC. There was statistically significant difference between all the materials at various time intervals. Conclusion: MTA Angelus showed superior sealing ability as a retrograde filling material followed by Biodentine and MTA Plus. PMID:29386776

Determination of Water Vapor Pressure Over Corrosive Chemicals Versus Temperature Using Raman Spectroscopy as Exemplified with 85.5% Phosphoric Acid.

PubMed

Rodier, Marion; Li, Qingfeng; Berg, Rolf Willestofte; Bjerrum, Niels Janniksen

2016-07-01

A method to determine the water vapor pressure over a corrosive substance was developed and tested with 85.5 ± 0.4% phosphoric acid. The water vapor pressure was obtained at a range of temperatures from ∼25 ℃ to ∼200 ℃ using Raman spectrometry. The acid was placed in an ampoule and sealed with a reference gas (either hydrogen or methane) at a known pressure (typically ∼0.5 bar). By comparing the Raman signals from the water vapor and the references, the water pressure was determined as a function of temperature. A considerable amount of data on the vapor pressure of phosphoric acid are available in the literature, to which our results could successfully be compared. A record value of the vapor pressure, 3.40 bar, was determined at 210 ℃. The method required a determination of the precise Raman scattering ratios between the substance, water, and the used reference gas, hydrogen or methane. In our case the scattering ratios between water and reference ν1 Q-branches were found to be 1.20 ± 0.03 and 0.40 ± 0.02 for H2 and CH4, respectively. © The Author(s) 2016.

Magnesium and cadmium containing Heusler phases REPd2Mg, REPd2Cd, REAg2Mg, REAu2Mg and REAu2Cd

NASA Astrophysics Data System (ADS)

Johnscher, Michael; Stein, Sebastian; Niehaus, Oliver; Benndorf, Christopher; Heletta, Lukas; Kersting, Marcel; Höting, Christoph; Eckert, Hellmut; Pöttgen, Rainer

2016-02-01

Twenty-eight new Heusler phases REPd2Mg, REPd2Cd, REAg2Mg, REAu2Mg and REAu2Cd with different rare earth elements were synthesized from the elements in sealed niobium ampoules in a water-cooled sample chamber of an induction furnace. The samples were characterized by powder X-ray diffraction. The cell volumes show the expected lanthanide contraction. The structures of YPd2Cd, GdPd2Cd, GdAu2Cd, Y1.12Ag2Mg0.88 and GdAg2Mg were refined based on single crystal diffractometer data. The magnetic properties were determined for fifteen phase pure samples. LuAu2Mg is a weak Pauli paramagnet with a susceptibility of 1.0(2) × 10-5 emu mol-1 at room temperature. The remaining samples show stable trivalent rare earth ions and most of them order magnetically at low temperatures. The ferromagnet GdAg2Mg shows the highest ordering temperature of TC = 98.3 K. 113Cd and 89Y MAS NMR spectra of YAu2Cd and YPd2Cd confirm the presence of unique crystallographic sites. The resonances are characterized by large Knight shifts, whose magnitude can be correlated with electronegativity trends.

Time Dependence of Tip Morphology during Cellular/Dendritic Arrayed Growth

NASA Technical Reports Server (NTRS)

Song, H.; Tewari, S. N.

1996-01-01

Succinonitrile-1.9 wt pct acetone has been directionally solidified in 0.7 X 0.7-cm-square cross section pyrex ampoules in order to observe the cell/dendrite tip morphologies, not influenced by the 'wall effects', which are present during growth in the generally used thin (about 200 gm) crucibles. The tips do not maintain a steady-state shape, as is generally assumed. Instead, they fluctuate within a shape envelope. The extent of fluctuation increases with decreasing growth speed, as the micro structure changes from the dendritic to cellular. The influence of natural convection has been examined by comparing these morphologies with those grown, without convection, in the thin ampoules.

Durability of Waste Glass Flax Fiber Reinforced Mortar

NASA Astrophysics Data System (ADS)

Aly, M.; Hashmi, M. S. J.; Olabi, A. G.; Messeiry, M.

2011-01-01

The main concern for natural fibre reinforced mortar composites is the durability of the fibres in the alkaline environment of cement. The composites may undergo a reduction in strength as a result of weakening of the fibres by a combination of alkali attack and fibre mineralisation. In order to enhance the durability of natural fiber reinforced cement composites several approaches have been studied including fiber impregnation, sealing of the matrix pore system and reduction of matrix alkalinity through the use of pozzolanic materials. In this study waste glass powder was used as a pozzolanic additive to improve the durability performance of flax fiber reinforced mortar (FFRM). The durability of the FFRM was studied by determining the effects of ageing in water and exposure to wetting and drying cycles; on the microstructures and flexural behaviour of the composites. The mortar tests demonstrated that the waste glass powder has significant effect on improving the durability of FFRM.

Silver nanocluster catalytic microreactors for water purification

NASA Astrophysics Data System (ADS)

Da Silva, B.; Habibi, M.; Ognier, S.; Schelcher, G.; Mostafavi-Amjad, J.; Khalesifard, H. R. M.; Tatoulian, M.; Bonn, D.

2016-07-01

A new method for the elaboration of a novel type of catalytic microsystem with a high specific area catalyst is developed. A silver nanocluster catalytic microreactor was elaborated by doping a soda-lime glass with a silver salt. By applying a high power laser beam to the glass, silver nanoclusters are obtained at one of the surfaces which were characterized by BET measurements and AFM. A microfluidic chip was obtained by sealing the silver coated glass with a NOA 81 microchannel. The catalytic activity of the silver nanoclusters was then tested for the efficiency of water purification by using catalytic ozonation to oxidize an organic pollutant. The silver nanoclusters were found to be very stable in the microreactor and efficiently oxidized the pollutant, in spite of the very short residence times in the microchannel. This opens the way to study catalytic reactions in microchannels without the need of introducing the catalyst as a powder or manufacturing complex packed bed microreactors.

A Microsystem Based on Porous Silicon-Glass Anodic Bonding for Gas and Liquid Optical Sensing

PubMed Central

De Stefano, Luca; Malecki, Krzysztof; Della Corte, Francesco G.; Moretti, Luigi; Rea, Ilaria; Rotiroti, Lucia; Rendina, Ivo

2006-01-01

We have recently presented an integrated silicon-glass opto-chemical sensor for lab-on-chip applications, based on porous silicon and anodic bonding technologies. In this work, we have optically characterized the sensor response on exposure to vapors of several organic compounds by means of reflectivity measurements. The interaction between the porous silicon, which acts as transducer layer, and the organic vapors fluxed into the glass sealed microchamber, is preserved by the fabrication process, resulting in optical path increase, due to the capillary condensation of the vapors into the pores. Using the Bruggemann theory, we have calculated the filled pores volume for each substance. The sensor dynamic has been described by time-resolved measurements: due to the analysis chamber miniaturization, the response time is only of 2 s. All these results have been compared with data acquired on the same PSi structure before the anodic bonding process.

Glass-ceramic joint and method of joining

DOEpatents

Meinhardt, Kerry D [Richland, WA; Vienna, John D [West Richland, WA; Armstrong, Timothy R [Clinton, TN; Pederson, Larry R [Kennewick, WA

2003-03-18

The present invention is a glass-ceramic material and method of making useful for joining a solid ceramic component and at least one other solid component. The material is a blend of M1-M2-M3, wherein M1 is BaO, SrO, CaO, MgO, or combinations thereof, M2 is Al.sub.2 O.sub.3, present in the blend in an amount from 2 to 15 mol %, M3 is SiO.sub.2 with up to 50 mol % B.sub.2 O.sub.3 that substantially matches a coefficient of thermal expansion of the solid electrolyte. According to the present invention, a series of glass ceramics in the M1-Al.sub.2 O.sub.3 -M3 system can be used to join or seal both tubular and planar solid oxide fuel cells, oxygen electrolyzers, and membrane reactors for the production of syngas, commodity chemicals and other products.

In-Situ Observation of Horizontal Centrifugal Casting using a High-Speed Camera

NASA Astrophysics Data System (ADS)

Esaka, Hisao; Kawai, Kohsuke; Kaneko, Hiroshi; Shinozuka, Kei

2012-07-01

In order to understand the solidification process of horizontal centrifugal casting, experimental equipment for in-situ observation using transparent organic substance has been constructed. Succinonitrile-1 mass% water alloy was filled in the round glass cell and the glass cell was completely sealed. To observe the movement of equiaxed grains more clearly and to understand the effect of movement of free surface, a high-speed camera has been installed on the equipment. The most advantageous point of this equipment is that the camera rotates with mold, so that one can observe the same location of the glass cell. Because the recording rate could be increased up to 250 frames per second, the quality of movie was dramatically modified and this made easier and more precise to pursue the certain equiaxed grain. The amplitude of oscillation of equiaxed grain ( = At) decreased as the solidification proceeded.

Ceramic composite coating

DOEpatents

Wicks, George G.

1997-01-01

A thin, room-temperature-curing, ceramic composite for coating and patching etal substrates comprises a sol gel silica glass matrix filled with finely ground particles or fibers, preferably alumina. The sol gel glass is made by adding ethanol to water to form a first mixture, then separately adding ethanol to tetraethyl orthosilicate to form a second mixture, then slowly adding the first to the second mixture to make a third mixture, and making a slurry by adding the finely ground particles or fibers to the third mixture. The composite can be applied by spraying, brushing or trowelling. If applied to patch fine cracks, densification of the ceramic composite may be obtained to enhance sealing by applying heat during curing.

Ceramic composite coating

DOEpatents

Wicks, G.G.

1997-01-21

A thin, room-temperature-curing, ceramic composite for coating and patching metal substrates comprises a sol gel silica glass matrix filled with finely ground particles or fibers, preferably alumina. The sol gel glass is made by adding ethanol to water to form a first mixture, then separately adding ethanol to tetraethyl orthosilicate to form a second mixture, then slowly adding the first to the second mixture to make a third mixture, and making a slurry by adding the finely ground particles or fibers to the third mixture. The composite can be applied by spraying, brushing or trowelling. If applied to patch fine cracks, densification of the ceramic composite may be obtained to enhance sealing by applying heat during curing.

MEMS for vibration energy harvesting

NASA Astrophysics Data System (ADS)

Li, Lin; Zhang, Yangjian; San, Haisheng; Guo, Yinbiao; Chen, Xuyuan

2008-03-01

In this paper, a capacitive vibration-to-electrical energy harvester was designed. An integrated process flow for fabricating the designed capacitive harvester is presented. For overcoming the disadvantage of depending on external power source in capacitive energy harvester, two parallel electrodes with different work functions are used as the two electrodes of the capacitor to generate a build-in voltage for initially charging the capacitor. The device is a sandwich structure of silicon layer in two glass layers with area of about 1 cm2. The silicon structure is fabricated by using silicon-on-insulator (SOI) wafer. The glass wafers are anodic bonded on to both sides of the SOI wafer to create a vacuum sealed package.

Monitoring Sealant Durability during Instrumented Outdoor Exposure with Variation in Prestrain

Treesearch

Gregory T. Schueneman; Steven Lacher; Christopher G. Hunt

2015-01-01

Sealants are a vital part of a building’s environmental barrier envelope. Their ability to bond to numerous dissimilar substrates and form cure-in-place seals results in their widespread use throughout single story and high rise buildings. A typical 40 story concrete and glass facade building can have 70 miles of sealant bonds. Failure of sealants can lead to energy...

Reliability Factors for Electronic Components in a Storage Environment

DTIC Science & Technology

1977-09-01

Other moisture-induced failure mechanisms include crack propagation in brittle materials such as ceramic seals, glass passivation layers, nitride ...for Aluminum -Gold .... .............. ... 80 4-5 Fatigue S-N Curve Typical for Most Metals and Polymers . 85 4-6 Comparison of Surface Damageý Within...8 Aluminum -Silicon Phase Diagram ...... ............... 96 5-1 Evaluation of Gases from Microcircuit Package .... ....... 121 6-1 Plot of Resistivity

Glass Solder Approach for Robust, Low-Loss, Fiber-to-Waveguide Coupling

NASA Technical Reports Server (NTRS)

McNeil, Shirley; Battle, Philip; Hawthorne, Todd; Lower, John; Wiley, Robert; Clark, Brett

2012-01-01

The key advantages of this approach include the fact that the index of interface glass (such as Pb glass n = 1.66) greatly reduces Fresnel losses at the fiber-to-waveguide interface, resulting in lower optical losses. A contiguous structure cannot be misaligned and readily lends itself for use on aircraft or space operation. The epoxy-free, fiber-to-waveguide interface provides an optically pure, sealed interface for low-loss, highpower coupling. Proof of concept of this approach has included successful attachment of the low-melting-temperature glass to the x-y plane of the crystal, successful attachment of the low-meltingtemperature glass to the end face of a standard SMF (single-mode fiber), and successful attachment of a wetted lowmelting- temperature glass SMF to the end face of a KTP crystal. There are many photonic components on the market whose performance and robustness could benefit from this coupling approach once fully developed. It can be used in a variety of fibercoupled waveguide-based components, such as frequency conversion modules, and amplitude and phase modulators. A robust, epoxy-free, contiguous optical interface lends itself to components that require low-loss, high-optical-power handling capability, and good performance in adverse environments such as flight or space operation.

Determination of tramadol hydrochloride in ampoule dosage forms by using UV spectrophotometric and HPLC-DAD methods in methanol and water media.

PubMed

Küçük, Aysel; Kadioğlu, Yücel

2005-02-01

Two newly developed simple and sensitive methods for determination of tramadol hydrochloride in ampoule dosage forms were described and validated. Measurements for spectrophotometric method were performed using UV-Vis Spectrophotometer in ranges of 200-400 nm. The solutions of standard and the samples were prepared in methanol and water media and the UV absorption spectrums of tramadol were monitored with maximum absorptions at 275 and 271 nm for both mediums, respectively. The standard calibration curves of tramadol were constructed by plotting absorbance vs. concentration in the concentration range with the final dilution of 10-100 microg ml-1. Reversed phase chromatography for HPLC method was conducted using a Phenomenex Bondclone C18 column with an isocratic mobile phase consisting of 25% acetonitrile in 75% 0.01 M phosphate buffer (pH 3). The effluent was monitored on a DAD detector at 218 nm. Linear response (r>0.99) was observed over the range of 0.5-40 microg ml-1 for methanol and water and run on six different occasions. The methods were applied successfully to pharmaceutical ampoule forms, but also for comparison in two different solvent media. Besides, it was completely validated and proven to be rugged.

Laser microjoining of dissimilar and biocompatible materials

NASA Astrophysics Data System (ADS)

Bauer, Ingo; Russek, Ulrich A.; Herfurth, Hans J.; Witte, Reiner; Heinemann, Stefan; Newaz, Golam; Mian, A.; Georgiev, D.; Auner, Gregory W.

2004-07-01

Micro-joining and hermetic sealing of dissimilar and biocompatible materials is a critical issue for a broad spectrum of products such as micro-electronics, micro-optical and biomedical products and devices. Today, biocompatible titanium is widely applied as a material for orthopedic implants as well as for the encapsulation of implantable devices such as pacemakers, defibrillators, and neural stimulator devices. Laser joining is the process of choice to hermetically seal such devices. Laser joining is a contact-free process, therefore minimizing mechanical load on the parts to be joined and the controlled heat input decreases the potential for thermal damage to the highly sensitive components. Laser joining also offers flexibility, shorter processing time and higher quality. However, novel biomedical products, in particular implantable microsystems currently under development, pose new challenges to the assembly and packaging process based on the higher level of integration, the small size of the device's features, and the type of materials and material combinations. In addition to metals, devices will also include glass, ceramic and polymers as biocompatible building materials that must be reliably joined in similar and dissimilar combinations. Since adhesives often lack long-term stability or do not meet biocompatibility requirements, new joining techniques are needed to address these joining challenges. Localized laser joining provides promising developments in this area. This paper describes the latest achievements in micro-joining of metallic and non-metallic materials with laser radiation. The focus is on material combinations of metal-polymer, polymer-glass, metal-glass and metal-ceramic using CO2, Nd:YAG and diode laser radiation. The potential for applications in the biomedical sector will be demonstrated.

Microgravity

NASA Image and Video Library

1992-04-24

Ampoule view of the Vapor Crystal Growth System (VCGS) Furnace. Used on IML-1 International Microgravity Laboratory Spacelab 3. Prinicipal Investigator and Payload Specialist was Lodewijk van den Berg.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

2003-01-01

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached- Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a method to make in situ pressure measurements in the growth ampoules.

Online drug information platform for the public in Hong Kong-Review of local drug information use and needs.

PubMed

Cheng, F W T; So, S W K; Fung, B W T; Hung, W H; Lee, V W Y

2018-06-01

In view of the popularity of Internet usage in Hong Kong, an interactive web-based drug information platform entitled "Ask My Pharmacist - Online University Led drug Enquiry Platform" (AMPOULE) was launched in 2009 to better serve the needs of drug information in Hong Kong. This paper aimed to evaluate the utility of AMPOULE in improving drug-related knowledge among the public and to reassess the needs of the general public in Hong Kong. All enquiries sent via AMPOULE were reviewed. Demographic data, nature of questions and types of drug class covered were analyzed. The workload of pharmacists was examined with respect to the preparation time needed for the enquiry, the lag days to reply and also the timing of enquiry recipient. 2122 enquiries were received from 2009 to 2017. Most enquirers were from Hong Kong (56.6%) and female gender (49.2%). 13% of the concerned subjects were aged over 61-year-old. The most frequent types of questions and medications covered were "Drug Ingredients and Indications" (28.0%) and Adverse Drug Reactions (26.8%) and "Cardiovascular Medication" (21.9%) respectively but these varied in different age groups or enquirer groups. The median time for preparation was 40.0 min (IQR: 25-65 min) while the median time lag was found to be 2.5 days (IQR: 1.0-5.0 days). The number of enquiries received was evenly distributed throughout the day except during 1:00 am to 9:00 am and 7:00 pm to 8:00 pm. AMPOULE has demonstrated that an online platform providing patient-oriented drug information service through the Internet is promising and further promotion is warranted. Current data suggested that the need of different age groups and enquirer groups are different and should therefore be individualized. Copyright © 2018 Elsevier B.V. All rights reserved.

Marginal adaptation and retention of a glass-ionomer, resin-modified glass-ionomers and a polyacid-modified resin composite in cervical Class-V lesions.

PubMed

Gladys, S; Van Meerbeek, B; Lambrechts, P; Vanherle, G

1998-07-01

An 18-month follow-up clinical trial of one conventional glass-ionomer (HIFI Master Palette), three resin-modified glass-ionomers (Fuji II LC, Vitremer, 3M Exp. 155) and one polyacid-modified resin composite (Dyract) was conducted to evaluate their clinical effectiveness in Class-V cervical lesions. In addition, the interface between dentin and two resin-modified glass-ionomers and one polyacid-modified resin composite was examined by scanning electron microscopy (SEM). After evaluation of the restorations immediately following placement (baseline), all patients were subjected to a strict recall schedule with controls at 6, 12 and 18 months. The clinical effectiveness was recorded in terms of retention and marginal integrity, clinical microleakage, caries recurrence, and tooth vitality. A chi 2-test (p < 0.05) was used to test for significant differences between materials. In case of restoration loss or special defects, a replica was made to examine the surface texture and restoration margins by SEM. In vitro, the interface was examined by SEM after an argon-ion-beam etching technique was used to enhance surface relief and disclose interfacial substructures. Retention appeared to be good for all the materials tested. Marginal discrepancies were localized at the incisal enamel and/or the cervical dentin margin, except for the polyacid-modified resin composite that showed most of the defects at the incisal enamel margin. None of the systems could guarantee margins free of microleakage for a long time. In vitro, the type of dentin pre-treatment defines to a great extent the morphology of the resultant interface between dentin and the restorative material tested. In this clinical study, the retention rate of the tested materials was good and even excellent for some products. Perfect marginal adaptation deteriorated too fast. The marginal adaptation of the polyacid-modified resin composite at the enamel site would probably have been better by the use of selective enamel or total acid etching. Marginal sealing remains a problem. Future research should concentrate on improving the marginal adaptation and sealing capacities before a broader clinical use can be advocated.

Clinical evaluation of glass ionomer for pit and fissure sealing of fully erupted molars.

PubMed

Sly, Edith G; Kaplan, Andrea E; Missana, Liliana

2010-01-01

The aim of this study was to evaluate the clinical behavior of two conventional glass ionomers used for pit and fissure sealing in terms of retention, marginal adaptation, caries recurrence and cracking. Eighty-three fully erupted first permanent molars were sealed, in a group of children aged 5 to 8 years. A double-blind, single operator, paired design was used. Materials applied were Fuji IX and VII. Retention (R), presence of caries (PC), marginal discoloration (MD), marginal adaptation (MA) and cracking (C) were evaluated at 6 and 12 months using Ryge's criteria. Data registered 6 months after treatment were: Fuji IX: R: Alpha 37, Bravo 2, Charlie: 4; PC: Alpha 43, Bravo: 0; MA: Alpha 38, Bravo: 1; MD: Alpha 39, Bravo: 0, Charlie: 0; C: Alpha 39, Bravo: 0. Fuji VII: R: Alpha 29, Bravo 4, Charlie: 7; PC: Alpha 40, Bravo: 0; MA: Alpha: 34, Bravo: 0; MD: Alpha: 34, Bravo: 0, Charlie: 0; C: Alpha 33, Bravo: 0. Results after one year were: Fuji IX: R: Alpha 33, Bravo: 3, Charlie: 9; PC: Alpha 44, Bravo: 1; MA: Alpha 33, Bravo: 1; MD: Alpha: 34, Bravo: 0, Charlie: 0; C: Alpha: 34, Bravo: 0. Fuji VII: R: Alpha 22, Bravo 4, Charlie: 13, PC: Alpha 40, Bravo: 0; MA: Alpha 23, Bravo: 1; MD: Alpha 23, Bravo: 1, Charlie: 0; C: Alpha 23, Bravo: 1. Statistical analysis using Fisher test showed no significant difference (p > 0.05) for R, and MA. For PC, MD and C, values are not reported because both materials showed the same results. The second control showed no significant difference (p > 0.05) for R, MA, PC, MD and C. Results suggest no difference between Fuji IX and Fuji VII as sealants in fully erupted permanent molars.

Light-addressable measurements of cellular oxygen consumption rates in microwell arrays based on phase-based phosphorescence lifetime detection

PubMed Central

Huang, Shih-Hao; Hsu, Yu-Hsuan; Wu, Chih-Wei; Wu, Chang-Jer

2012-01-01

A digital light modulation system that utilizes a modified commercial digital micromirror device (DMD) projector, which is equipped with a UV light-emitting diode as a light modulation source, has been developed to spatially direct excited light toward a microwell array device to detect the oxygen consumption rate (OCR) of single cells via phase-based phosphorescence lifetime detection. The microwell array device is composed of a combination of two components: an array of glass microwells containing Pt(II) octaethylporphine (PtOEP) as the oxygen-sensitive luminescent layer and a microfluidic module with pneumatically actuated glass lids set above the microwells to controllably seal the microwells of interest. By controlling the illumination pattern on the DMD, the modulated excitation light can be spatially projected to only excite the sealed microwell for cellular OCR measurements. The OCR of baby hamster kidney-21 fibroblast cells cultivated on the PtOEP layer within a sealed microwell has been successfully measured at 104 ± 2.96 amol s−1 cell−1. Repeatable and consistent measurements indicate that the oxygen measurements did not adversely affect the physiological state of the measured cells. The OCR of the cells exhibited a good linear relationship with the diameter of the microwells, ranging from 400 to 1000 μm and containing approximately 480 to 1200 cells within a microwell. In addition, the OCR variation of single cells in situ infected by Dengue virus with a different multiplicity of infection was also successfully measured in real-time. This proposed platform provides the potential for a wide range of biological applications in cell-based biosensing, toxicology, and drug discovery. PMID:24348889

Sacrificial adhesive bonding: a powerful method for fabrication of glass microchips

PubMed Central

Lima, Renato S.; Leão, Paulo A. G. C.; Piazzetta, Maria H. O.; Monteiro, Alessandra M.; Shiroma, Leandro Y.; Gobbi, Angelo L.; Carrilho, Emanuel

2015-01-01

A new protocol for fabrication of glass microchips is addressed in this research paper. Initially, the method involves the use of an uncured SU-8 intermediate to seal two glass slides irreversibly as in conventional adhesive bonding-based approaches. Subsequently, an additional step removes the adhesive layer from the channels. This step relies on a selective development to remove the SU-8 only inside the microchannel, generating glass-like surface properties as demonstrated by specific tests. Named sacrificial adhesive layer (SAB), the protocol meets the requirements of an ideal microfabrication technique such as throughput, relatively low cost, feasibility for ultra large-scale integration (ULSI), and high adhesion strength, supporting pressures on the order of 5 MPa. Furthermore, SAB eliminates the use of high temperature, pressure, or potential, enabling the deposition of thin films for electrical or electrochemical experiments. Finally, the SAB protocol is an improvement on SU-8-based bondings described in the literature. Aspects such as substrate/resist adherence, formation of bubbles, and thermal stress were effectively solved by using simple and inexpensive alternatives. PMID:26293346

Moisture ingress prediction in polyisobutylene-based edge seal with molecular sieve desiccant

DOE PAGES

Kempe, Michael D.; Nobles, Dylan L.; Postak, Lori; ...

2017-10-26

Often photovoltaic modules are constructed with materials that are sensitive to water. This is most often the case with thin film technologies, including perovskite cells, where the active layers are a few microns thick and can be sensitive to moisture, liquid water or both. When moisture or liquid water can ingress, a small amount of water can lead to corrosion and depending on the resulting reactions, a larger local detrimental effect is possible. To prevent moisture from contacting photovoltaic components, impermeable frontsheets and backsheets are used with a polyisobutylene (PIB)-based edge seal material around the perimeter. Here, we evaluate themore » ability of a PIB-based edge seal using a molecular sieve desiccant to keep moisture out for the expected module lifetime. Moisture ingress is evaluated using test coupons where the edge seal is placed between 2 pieces of glass, one of which has a metallic calcium film on it, and monitoring the moisture ingress distance as a function of time. We expose samples to different temperature and humidity conditions to create permeation models useful for extrapolation to field use. This extrapolation indicates that this PIB material is capable of keeping moisture out of a module for the desired lifetime.« less

Moisture ingress prediction in polyisobutylene-based edge seal with molecular sieve desiccant

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kempe, Michael D.; Nobles, Dylan L.; Postak, Lori

Often photovoltaic modules are constructed with materials that are sensitive to water. This is most often the case with thin film technologies, including perovskite cells, where the active layers are a few microns thick and can be sensitive to moisture, liquid water or both. When moisture or liquid water can ingress, a small amount of water can lead to corrosion and depending on the resulting reactions, a larger local detrimental effect is possible. To prevent moisture from contacting photovoltaic components, impermeable frontsheets and backsheets are used with a polyisobutylene (PIB)-based edge seal material around the perimeter. Here, we evaluate themore » ability of a PIB-based edge seal using a molecular sieve desiccant to keep moisture out for the expected module lifetime. Moisture ingress is evaluated using test coupons where the edge seal is placed between 2 pieces of glass, one of which has a metallic calcium film on it, and monitoring the moisture ingress distance as a function of time. We expose samples to different temperature and humidity conditions to create permeation models useful for extrapolation to field use. This extrapolation indicates that this PIB material is capable of keeping moisture out of a module for the desired lifetime.« less

Evaluation of time required for recontamination of coronally sealed canals medicated with calcium hydroxide and chlorhexidine.

PubMed

Gomes, B P F A; Sato, E; Ferraz, C C R; Teixeira, F B; Zaia, A A; Souza-Filho, F J

2003-09-01

To determine in vitro the time required for recontamination of coronally sealed canals medicated with either calcium hydroxide (CaOH2), 2% chlorhexidine gel (CG) or with a combination of both. Eighty intact, caries-free, premolar teeth with straight roots and mature apices were selected for the study. After biomechanical preparation of 75 teeth, they were randomly divided into nine groups according to the intracanal medicament and the coronal seal with 'Intermediate Restorative Material' (IRM) as follows: (i) 10 teeth medicated with CG, coronally unsealed; (ii) 10 teeth medicated with CaOH2, coronally unsealed; (iii) 10 teeth medicated with CaOH2 + CG, coronally unsealed; (iv) 10 teeth medicated with CG + coronal seal; (v) 10 teeth medicated with CaOH2 + coronal seal; (vi) 10 teeth medicated with CG + CaOH2 + coronal seal; (vii) 10 teeth without intracanal medicament and coronally sealed; (viii) 5 teeth without intracanal medicament and coronally unsealed, used as the positive control group (PC); (ix) 5 teeth with intact crowns used as the negative control group (NC). Glass flasks were filled with Brain Heart Infusion broth (BHI), so that only the root apex was in contact with the broth, while the crown was immersed in human saliva + BHI (3:1). The flasks were then incubated at 37 degrees C in an atmosphere of 10% CO2, and microbial growth was checked daily. All specimens of the PC showed contamination within 1 day of incubation, while the NC showed no evidence of broth turbidity. Recontamination was detected after an average time of 3.7 days in the unsealed canals medicated with CG, 1.8 days in the group medicated with CaOH2 and 2.6 days in the group medicated with CaOH2 + CG. When the crowns were sealed with IRM, recontamination was detected within 13.5 days in the canals medicated with CG, after 17.2 days in the group medicated with CaOH2 and after 11.9 days in the group medicated with CG + CaOH2. The group with no medication, but sealed with IRM, showed recontamination after 8.7 days. There were statistically significant differences between the teeth with or without coronal seal (P<0.05). The coronal seal delayed but did not prevent leakage of microorganisms. There was no difference between the various medicaments.

Tunable-focus liquid lens controlled using a servo motor

NASA Astrophysics Data System (ADS)

Ren, Hongwen; Fox, David; Anderson, P. Andrew; Wu, Benjamin; Wu, Shin-Tson

2006-09-01

We demonstrated a liquid lens whose focal length can be controlled by an actuator. The lens cell is composed of elastic membrane, planar glass plate, a periphery sealing ring, and a liquid with a fixed volume in the lens chamber. Part of the periphery sealing ring is excavated to form a hollow chamber which functions as a reservoir. This hollowed periphery is surrounded by an exterior rubber membrane. The shaft of an actuator is used to deform the elastic rubber. Squeezing the liquid contained in the reservoir into the lens chamber. Excess liquid in the lens chamber will push the lens membrane to outward, resulting in a lens shape change. Due to the compact structure and easy operation, this liquid lens has potential applications in zoom lenses, auto beam steering, and eyeglasses.

Development of NASA's Sample Cartridge Assembly: Summary of GEDS Design, Development Testing, and Thermal Analyses

NASA Technical Reports Server (NTRS)

O'Connor, Brian; Hernandez, Deborah; Hornsby, Linda; Brown, Maria; Horton-Mullins, Kathryn

2017-01-01

Outline: Background of ISS (International Space Station) Material Science Research Rack; NASA SCA (Sample Cartridge Assembly) Design; GEDS (Gravitational Effects in Distortion in Sintering) Experiment Ampoule Design; Development Testing Summary; Thermal Modeling and Analysis. Summary: GEDS design development challenging (GEDS Ampoule design developed through MUGS (Microgravity) testing; Short duration transient sample processing; Unable to measure sample temperatures); MUGS Development testing used to gather data (Actual LGF (Low Gradient Furnace)-like furnace response; Provided sample for sintering evaluation); Transient thermal model integral to successful GEDS experiment (Development testing provided furnace response; PI (Performance Indicator) evaluation of sintering anchored model evaluation of processing durations; Thermal transient model used to determine flight SCA sample processing profiles).

Identification and Quantification of Hydrocarbon Products in Effluents.

DTIC Science & Technology

1980-05-01

Tobyhanna Army Depot ATTN: Const. Mgmt. Br. Jacksonville Tooele Army Depot ATTN: Engr. Library Japan Watervliet Arsenal Jidda Yuma Proving Ground Chief...the prepared standard series were stored in volumetric flasks sealed with latex caps over ground glass stoppers. Absorption spectra of the standa-rds in...Facilities Engineer Walter Reed Army Medical Center ATTN: DAEN-CW ARRADCOM ATIN: DAEN-RM Aberdeen Proving Ground USACC ATTN: DAEN-CCP Army Matis. and Mechanics

Optical temperature sensor using thermochromic semiconductors

DOEpatents

Kronberg, James W.

1996-01-01

An optical temperature measuring device utilizes thermochromic semiconductors which vary in color in response to changes in temperature. The thermochromic material is sealed in a glass matrix which allows the temperature sensor to detect high temperatures without breakdown. Cuprous oxide and cadmium sulfide are among the semiconductor materials which provide the best results. The changes in color may be detected visually or by utilizing an optical fiber and an electrical sensing circuit.

Optical temperature sensor using thermochromic semiconductors

DOEpatents

Kronberg, James W.

1998-01-01

An optical temperature measuring device utilizes thermochromic semiconductors which vary in color in response to changes in temperature. The thermochromic material is sealed in a glass matrix which allows the temperature sensor to detect high temperatures without breakdown. Cuprous oxide and cadmium sulfide are among the semiconductor materials which provide the best results. The changes in color may be detected visually using a sensor chip and an accompanying color card.

Environmental Effects on Spacecraft Material

DTIC Science & Technology

1988-05-01

degradation. The solar cell panels and adhesives used are vulnerable, as are various metal mirrors . Overcoats of SiO 2 limit the erosion due to atomic oxygen if...components (insulation, seals, lubricants, mirrors , etc.) are being studied. The Johnson Spaceflight Center is also the center of research on...fused silica, ULE (Ultra Low Expansion) and a glass ceramic, Zerodur . The results of the facility visits confirmed the results of the question

Optical temperature sensor using thermochromic semiconductors

DOEpatents

Kronberg, J.W.

1998-06-30

An optical temperature measuring device utilizes thermochromic semiconductors which vary in color in response to changes in temperature. The thermochromic material is sealed in a glass matrix which allows the temperature sensor to detect high temperatures without breakdown. Cuprous oxide and cadmium sulfide are among the semiconductor materials which provide the best results. The changes in color may be detected visually using a sensor chip and an accompanying color card. 8 figs.

Resonant acoustic measurement of vapor phase transport phenomenon in porous media

NASA Astrophysics Data System (ADS)

Schuhmann, Richard; Garrett, Steven

2002-05-01

Diffusion of gases through porous media is commonly described using Fick's law and is characterized by a gas diffusion coefficient modified by a media-specific tortuosity parameter. A phase-locked-loop resonance frequency tracker [J. Acoust. Soc. Am. 108, 2520 (2000)] has been upgraded with an insulated copper resonator and a bellows-sealed piston instrumented with an accelerometer. Average system stability (temperature divided by frequency squared) is about 180 ppm. Glass-bead-filled cores of different lengths are fitted into an o-ring sealed opening at the top of the resonator. The rate at which the tracer gas is replaced by air within the resonator is controlled by the core's diffusion constant. Mean molecular weight of the gas mixture in the resonator is determined in real time from the ratio of the absolute temperature to the square of the fundamental acoustic resonance frequency. Molecular weight of the gas mixture is determined approximately six times per minute. Changes in the gas mixture concentration are exponential in time (within 0.1%) over nearly two decades in concentration. We will report diffusion constants for two different sizes of glass beads, in samples of five different lengths, using two different tracer gases, to establish the validity of this approach. [Work supported by ONR.

Phytotoxicity, uptake and metabolism of 1,4-dichlorobenzene by plant cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, M.J.; Bokern, M.; Boehme, C.

1996-07-01

Phytotoxicity, uptake, and metabolism of 1,4-dichlorobenzene (1,4-DCB) by carrot (Daucus carota L.), soybean (Glycine max. L.), tomato (Lycopersicon esculentum Mill.), and red goosefoot (Chenopodiun rubrum L.) cell suspension cultures were studied. Sealed glass systems were utilized for the investigation because 1,4-DCB is volatile. The sealed systems affect the growth of plant cells, but do not provide different results when testing xenobiotic uptake and metabolism. 1,4-Dichlorobenzene (40 {micro}g in 40 ml medium) was taken up by carrot (49%), soybean (50%), and red goosefoot (62%) cells. Only the soybean cell cultures provided evidence of the existence of metabolites of this compound, probablymore » conjugates of chlorophenols. Conditions for phytotoxicity tests were modified because the growth of cell cultures was affected when sealed for longer than 2 d. 1,4-Dichlorobenzene is toxic to cell cultures of the three tested plant species (tomato, soybean, and carrot). Concentrations of 0.5 mM caused 50% growth inhibition in carrot and soybean cultures. The tomato cultures were more sensitive, with 0.05 mM causing 50% growth inhibition.« less

Improved Gas Filling and Sealing of an HC-PCF

NASA Technical Reports Server (NTRS)

Poberezhskiy, Ilya; Meras, Patrick; Chang, Daniel; Spiers, Gary

2008-01-01

An improved packaging approach has been devised for filling a hollow-core photonic-crystal fiber (HC-PCF) with a gas, sealing the HC-PCF to retain the gas, and providing for optical connections and, optionally, a plumbing fitting for changing or augmenting the gas filling. Gas-filled HC-PCFs can be many meters long and have been found to be attractive as relatively compact, lightweight, rugged alternatives to conventional gas-filled glass cells for use as molecular-resonance frequency references for stabilization of lasers in some optical-metrology, lidar, optical-communication, and other advanced applications. Prior approaches to gas filling and sealing of HC-PCFs have involved, variously, omission of any attempt to connectorize the PCF, connectorization inside a vacuum chamber (an awkward and expensive process), or temporary exposure of one end of an HC-PCF to the atmosphere, potentially resulting in contamination of the gas filling. Prior approaches have also involved, variously, fusion splicing of HC-PCFs with other optical fibers or other termination techniques that give rise to Fresnel reflections of about 4 percent, which results in output intensity noise.

Comparative risk assessments for the production and interim storage of glass and ceramic waste forms: Defense waste processing facility

NASA Astrophysics Data System (ADS)

Huang, J. C.; Wright, W. V.

1982-04-01

The Defense Waste Processing Facility (DWPF) for immobilizing nuclear high level waste (HLW) is scheduled to be built. High level waste is produced when reactor components are subjected to chemical separation operations. Two candidates for immobilizing this HLW are borosilicate glass and crystalline ceramic, either being contained in weld sealed stainless steel canisters. A number of technical analyses are being conducted to support a selection between these two waste forms. The risks associated with the manufacture and interim storage of these two forms in the DWPF are compared. Process information used in the risk analysis was taken primarily from a DWPF processibility analysis. The DWPF environmental analysis provided much of the necessary environmental information.

Use of Glass Reinforced Concrete (GRC) as a substrate for photovoltaic modules

NASA Technical Reports Server (NTRS)

Eirls, J. L.

1980-01-01

A substrate for flat plate photovoltaic solar panel arrays using a glass fiber reinforced concrete (GRC) material was developed. The installed cost of this GRC panel is 30% less than the cost goal of the Near Term Low-Cost Flat Plate Photovoltaic Solar Array Program. The 4 ft by 8 ft panel is fabricated from readily available inexpensive materials, weighs a nominal 190 lbs., has exceptionally good strength and durability properties (rigid and resists weathering), is amenable to mass production and is easily installed on simple mountings. Solar cells are encapsulated in ethylene/vinyl acetate with Tedlar backing and Korad cover film. The laminates are attached to the GRC substrate with acrylic transfer tape and edge sealed with silicone RTV adhesive.

Apparatus for ultrasonic nebulization

DOEpatents

Olson, Kenneth W.; Haas, Jr., William J.; Fassel, Velmer A.

1978-08-29

An improved apparatus for ultrasonic nebulization of liquid samples or suspensions in which the piezoelectric transducer is protected from chemical attack and erosion. The transducer is protected by being bonded to the inner surface of a glass plate which forms one end wall of a first hollow body provided with apparatus for circulating a fluid for cooling and stabilizing the transducer. The glass plate, which is one-half wavelength in thickness to provide an acoustically coupled outer nebulizing surface, seals an opening in a second hollow body which encloses an aerosol mixing chamber. The second body includes apparatus for delivering the sample solution to the nebulizing surface, a gas inlet for providing a flow of carrier gas for transporting the aerosol of the nebulized sample and an aerosol outlet.

Growth rates and interface shapes in germanium and lead tin telluride observed in-situ, real-time in vertical Bridgman furnaces

NASA Technical Reports Server (NTRS)

Barber, P. G.; Berry, R. F.; Debnam, W. J.; Fripp, A. L.; Woodell, G.; Simchick, R. T.

1995-01-01

Using the advanced technology developed to visualize the melt-solid interface in low Prandtl number materials, crystal growth rates and interface shapes have been measured in germanium and lead tin telluride semiconductors grown in vertical Bridgman furnaces. The experimental importance of using in-situ, real time observations to determine interface shapes, to measure crystal growth rates, and to improve furnace and ampoule designs is demonstrated. The interface shapes observed in-situ, in real-time were verified by quenching and mechanically induced interface demarcation, and they were also confirmed using machined models to ascertain the absence of geometric distortions. Interface shapes depended upon the interface position in the furnace insulation zone, varied with the nature of the crystal being grown, and were dependent on the extent of transition zones at the ends of the ampoule. Actual growth rates varied significantly from the constant translation rate in response to the thermophysical properties of the crystal and its melt and the thermal conditions existing in the furnace at the interface. In the elemental semiconductor germanium the observed rates of crystal growth exceeded the imposed translation rate, but in the compound semiconductor lead tin telluride the observed rates of growth were less than the translation rate. Finally, the extent of ampoule thermal loading influenced the interface positions, the shapes, and the growth rates.

Influence of Applied Thermal Gradients and a Static Magnetic Field on Bridgman-Grown GeSi Alloys

NASA Technical Reports Server (NTRS)

Volz, M. P.; Szofran, F. R.; Cobb, S. D.; Ritter, T. M.

1999-01-01

The effect of applied axial and radial thermal gradients and an axial static magnetic field on the macrosegregation profiles of Bridgman-grown GeSi alloy crystals has been assessed. The axial thermal gradients were adjusted by changing the control setpoints of a seven-zone vertical Bridgman furnace. The radial thermal gradients were affected by growing samples in ampoules with different thermal conductivities, namely graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN). Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. All of the samples were grown on Ge seeds. This resulted in a period of free growth until the Si concentration in the solid was in equilibrium with the Si concentration in the liquid. The length of crystal grown during this period was inversely proportional to the applied axial thermal gradient. Several samples were grown in an axial 5 Tesla magnetic field. Measured macroscopic segregation profiles on these samples indicate that the magnetic field did not, in general, reduce the melt flow velocities to below the growth velocities.

SQUID measurements of remanent magnetisation in refillable 3He spin-filter cells (SFC)

NASA Astrophysics Data System (ADS)

Hutanu, V.; Rupp, A.; Sander-Thömmes, T.

2007-07-01

A strong influence of external magnetic fields on the relaxation time constant T1 of glass cells serving as reservoirs for polarised 3He, observed for various alkali metal-coated cells made of different glass types, was initially associated with the presence of a large number of ferromagnetic clusters on the glass surface. Later experiments showed the presence of the so-called “ T1 hysteresis” phenomenon with a similar distinctiveness also in uncoated cells made of pure synthetic quartz glass. It suggests that the origin of such a relaxation is a macroscopic magnetisation in the bulk of the cell. We present the results of a multi-SQUID system investigation on magnetised and non-magnetised quartz glass cells, Cs coated as well as bare wall, to be used as neutron spin filters at HMI Berlin. The presence of a macroscopic remanent magnetic moment in the cells after their exposition to external magnetic fields has been experimentally shown. More than 80% of the remanent magnetic moment of the magnetised cells was found to be concentrated in the region of the glass valves. SQUID measurements reveal the existence of some remanent magnetisation in all valve parts and also in the vacuum grease, but most magnetic are the plastic parts and the O-ring. Different valve and sealing types have been compared in order to find the less magnetisable one.

Study of structural, electrical, and dielectric properties of phosphate-borate glasses and glass-ceramics

NASA Astrophysics Data System (ADS)

Melo, B. M. G.; Graça, M. P. F.; Prezas, P. R.; Valente, M. A.; Almeida, A. F.; Freire, F. N. A.; Bih, L.

2016-08-01

In this work, phosphate-borate based glasses with molar composition 20.7P2O5-17.2Nb2O5-13.8WO3-34.5A2O-13.8B2O3, where A = Li, Na, and K, were prepared by the melt quenching technique. The as-prepared glasses were heat-treated in air at 800 °C for 4 h, which led to the formation of glass-ceramics. These high chemical and thermal stability glasses are good candidates for several applications such as fast ionic conductors, semiconductors, photonic materials, electrolytes, hermetic seals, rare-earth ion host solid lasers, and biomedical materials. The present work endorses the analysis of the electrical conductivity of the as-grown samples, and also the electrical, dielectric, and structural changes established by the heat-treatment process. The structure of the samples was analyzed using X-Ray powder Diffraction (XRD), Raman spectroscopy, and density measurements. Both XRD and Raman analysis confirmed crystals formation through the heat-treatment process. The electrical ac and dc conductivities, σac and σdc, respectively, and impedance spectroscopy measurements as function of the temperature, varying from 200 to 380 K, were investigated for the as-grown and heat-treated samples. The impedance spectroscopy was measured in the frequency range of 100 Hz-1 MHz.

Glass ionomer ART sealants in Chinese school children-6-year results.

PubMed

Holmgren, Christopher J; Lo, Edward C M; Hu, Deyu

2013-09-01

To evaluate longitudinally ART sealants placed in Chinese school children under field conditions. 191 ART sealants were placed in 140 children, aged 11-14 years, by five assistant dentists in four secondary schools in Deyang, Sichuan Province, China. Teeth selected for sealing were those with pits and fissures that were deep or showing early enamel caries. Teeth were excluded if there was obvious cavitation extending into dentine. Standard instruments and procedures for ART sealants were used. The material used was a high-viscosity glass-ionomer (Ketac-Molar, 3MESPE) that was inserted into the pits and fissures with the "press-finger" technique. The status of the sealants was evaluated annually over 6 years after placement by the same examiner who was not involved in the placement of the sealants using explorers, mouth-mirrors and an intra-oral fibre-optic light. No missing sealants were replaced during the study. 107 sealants (56% of the original) were examined after 6 years. The cumulative survival rates of the sealants (partially or fully retained) after 2, 4 and 6 years were 79%, 68% and 59%, respectively. Caries prevention lagged the fall in sealant survival but remained high throughout the study period, being over 90% in the first 4 years and 85% after 6 years. ART sealants placed under field conditions in Chinese schoolchildren have a high retention rate. Missing sealants should be replaced to maintain their preventive efficacy. The sealing of pits and fissures can be an effective caries preventive approach. Resin-based sealants have the disadvantage in that they require an optimal level of moisture control during placement. In children and in outreach situations glass ionomer ART sealants, which are more moisture tolerant, can offer a viable alternative. Copyright © 2013 Elsevier Ltd. All rights reserved.

Smart glass based on electrochromic polymers

NASA Astrophysics Data System (ADS)

Xu, Chunye; Kong, Xiangxing; Liu, Lu; Su, Fengyu; Kim, Sooyeun; Taya, Minoru

2006-03-01

Five-layer-structured electrochromic glass (window), containing a transparent conductive layer, an electrochromic layer, an ionic conductive layer, an ionic storage layer and a second conductive transparent layer, was fabricated. The electrochromic glass adopts the conjugated polymer, poly[3,3-dimethyl-3,4-dihydro-2H-thieno[3,4-b][1,4]dioxepine] (PProDOT-Me2), as a blue electrochromic active layer, vanadium pentaoxide film as an ion storage layer and polymer gel electrolyte as the ionic transport layer. Dimension of smart glass up to 12 x 20 inch was developed. UV curable sealant was applied for the sealing devices. Color changing or switching speed of 12 x 20 inch smart glass from dark state to the transparent state (or vise versa) is less than 15 seconds under applied 1.5 voltages. Besides the long open circuit memory (the colored state or transparent state remains the same state after the power is off), the smart window can be adjusted easily into the intermediate state between the dark state and the transparent state by just simply turn the power on or off. No space consuming or dirt collecting shades, curtains or blinds are needed. The applications of the smart window, e.g. in the aircrafts, automobiles and architectures were discussed as well.

Cyclic growth and dissolution of camphor crystals in quinary, ternary, and binary solutions: A study on crystal behavior in storm glass

NASA Astrophysics Data System (ADS)

Mitsuya, Takuro; Takahashi, Kyohei; Nagashima, Kazushige

2014-09-01

"Storm glass" is a hermetically sealed glass tube containing a solution of camphor. In 19th-century England, the pattern and quantity of the crystals were observed and interpreted as a weather forecasting tool. In the present study, the appearance of camphor crystals under cyclic temperature change was studied in three sample solutions, the storm glass solution (quinary system), camphor-ethanol-water (ternary system), and camphor-ethanol (binary system), to elucidate the effect of components in the storm glass on the appearance of camphor crystals. Equilibrium temperatures of camphor crystals as a function of the camphor concentration were also obtained to estimate the quantity of camphor crystals precipitated in the solutions. During the temperature cycles, the crystal height increased and decreased. The ranges (local maxima and minima) of crystal heights gradually decreased to approximately a constant range. Not only the crystal height but also the amplitude of the height variation in the quinary and ternary systems were much larger than those in the binary system, although the estimated weights of crystals precipitated in the quinary and ternary systems were smaller than that in the binary system. This fact resulted from the formation of dendrites in the quinary and ternary systems, which caused high porosity of sedimented crystals.

Commercialization Plan Support for Development of Low Cost Vacuum Insulating Glazing: Cooperative Research and Development Final Report, CRADA Number CRD-11-449

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dameron, Arrelaine

During the duration of this CRADA, V-Glass and NREL will partner in testing, analysis, performance forecasting, costing, and evaluation of V-Glass’s GRIPWELD™ process technology for creating a low cost hermetic seal for conventional and vacuum glazing. Upon successful evaluation of hermeticity, V-Glass’s GRIPWELD™ will be evaluated for its potential use in highly insulating window glazing.

Evaluation of Glider Coatings Against Biofouling for Improved Flight Performance

DTIC Science & Technology

2011-08-17

and used to conduct assays of survivorship with approximately 100 nauplii larvae ofArtemia sp. (brine shrimp ). The larvae were exposed to the...seal (D). These coatings showed higher mortality of brine shrimp as well as 100% mortality of cypris larvae during the settlement assay which...brine shrimp compared to the glass control; however these did not inhibit settlement and were evidently not toxic to the cypris larvae . All other

Thermal-desorption measurements for estimating bakeout characteristics of vacuum devices

NASA Astrophysics Data System (ADS)

Beavis, L.

1981-11-01

This discussion will be confined to outgassing phenomena; although gettering (sinks) or permeation (transfer through the entire vacuum wall) are imported in long term prediction. Measuring outgassing rates directly is complicated by the dynamic interaction between the samples being measured and the apparatus in which the measurements are made. Thermoesorption data are presented for molybdenum, nickel, Fe-Ni-Co alloy, copper, Cu-Be alloy, molybdenum sealing glass ceramic, and high-alumina ceramic.

Optical temperature sensor using thermochromic semiconductors

DOEpatents

Kronberg, J.W.

1996-08-20

An optical temperature measuring device utilizes thermochromic semiconductors which vary in color in response to changes in temperature. The thermochromic material is sealed in a glass matrix which allows the temperature sensor to detect high temperatures without breakdown. Cuprous oxide and cadmium sulfide are among the semiconductor materials which provide the best results. The changes in color may be detected visually or by utilizing an optical fiber and an electrical sensing circuit. 7 figs.

JPL encapsulation task

NASA Technical Reports Server (NTRS)

Willis, P.

1986-01-01

A detailed summary of the diverse encapsulation materials and techniques that evolved to meet the cost goals of the Flat-plate Solar Array (FSA) Project is presented. A typical solar cell now consists of low iron glass, two layers of ethylene vinyl acetate (EVA) polymers, a porous space, primers/adhesives, a back cover of Tedlar, and a gasket/seal for a volume cost of $1.30/sq ft. This compares well with the project goal of $1.40/sq ft.