Denton Discovery™ 18

RESEARCH/RESEARCHERS

Synthesis of Layered LiMnO2 Holds Potential asan Electrode for Rechargeable Lithium Batteries

Researchers at the University of St. Andrews, United Kingdom,reported the synthesis and performance of layered, anhydrous andstoichiometric LiMnQ2 as an electrode for rechargeable lithium bat-teries. They created the material by ion exchange from NaMnO2.The researchers, A. Robert Armstrong and Peter G. Bruce, reportedin the June 9 issue of Nature that they have obtained LiMnO2 byrefluxing NaMnO2 with an excess of LiCl or LiBr in n-hexanol at145-150°C for 6-8 hours. After cooling to room temperature theyfiltered the product under suction and washed it, first with n-hexa-nol and then with ethanol, then dried it. They established phasepurity by powder x-ray diffraction. The oxide ions are stacked incubic close-packed layers. Manganese ions reside in each octahe-dral site between the first and second oxide layers, and Li+ ionsbetween the second and third layers. According to the researchers,"up to 0.95 lithiums per formula unit may be extracted fromLiMnC^ on initial charging, corresponding to a capacity of 270 mAh g"1." At a current density of 0.5 mA cm"2, a capacity of 200 mA h g-1

may be reached up to a cut-off potential of 4.3 V.

Thin-Film Zirconia Electrolyte Doubles Fuel CellPerformance at 800°C

Focusing on solid oxide fuel cells (SOFCs), researchers at ErnestOrlando Lawrence Berkeley National Laboratory (Berkeley Lab)have used a ceramic process to develop a thin-film electrolyte thatboth doubles the current power output and significantly reducesthe cost of SOFCs.

The researchers report that cells with the ultra-thin ceramicelectrolyte generate 2 W/cm2 of cell surface area. During testing,the electrical output remains constant over 700 hours.

The electrolyte, a yttria-stabilized zirconia film, starts out as aceramic powder suspended in solution. The solution is paintedonto the anode (electrode) and then fired or sintered. The processreadily lends itself to assembly line usage. The anode that is paint-ed must be porous in order to'allow for the flow of hydrogen.Paints want to fill and plug up these pores rather than to sit on topof the porous anode. When the anode and ceramic coat are sin-tered, both shrink. Unless they shrink in unison, the ceramic cracksor pinholes form.

SOFCs have been most fuel-efficient operating at 1000°C. Thishigh temperature increases the cost of materials and decreases thelifetime of the cell. According to one of the researchers, Selmar deSouza, "SOFCs are solid-state devices. We know how to drop theiroperating temperature but the problem has been the electrolyte. Itconducts ions between electrodes and when you drop the temper-ature, you lose conductivity. One way to deal with this is by mak-ing the electrolyte thinner."

Institute of Materials Announces 1996 AwardsThe Institute of Materials awarded nearly 30 medals and prizes

for outstanding achievement in the field of engineered materials,given at the Institute's Annual General Meeting held in London onJune 5,1996. Among the recipients are, for the Griffith Silver Medaland Prize, A.J. Kinloch of Imperial College, a pioneer in using frac-ture mechanics in the analysis of adhesion; for the SwinburneAward, E.J. Kramer of Cornell University, a 25-year contributor tothe understanding of polymer physics; for the Platinum Medal,D.R.F. West of Imperial College whose main interests have beenalloy constitution, phase equilibria, phase transformation, and struc-ture/ property relationships; and for Honorary Fellowship of TheInstitute of Materials, D. McLean, in recognition of his lifetime con-tribution to physical metallurgy.

The following awards were given for personal achievements

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and outstanding papers: The GuyBengough Medal & Prize to A.M. Beccariaand G. Piggi of Instituto per la CorrosioneMarina dei Metalli; the Colclough Medal& Prize to G. Walker of British Steel,Scunthorpe Works; the Cook Prize to S.C.Flood of Powdrex Limited and P.A.Davidson of Cambridge University; theDowding Medal & Prize to J.L. Evans,consultant to British Steel; the ElegantWork Prize to P.D. Brown and C.J.Humphreys of the University ofCambridge; the Grunfeld Medal & Prize toL. Christodoulou of Imperial College; theHadfield Medal & Prize to R.N. Younger,formerly Technical Director, Davy Interna-tional; the Hancock Medal to D.A. Hills,consultant; the Hume Rothery Prize to L.Kaufman of Cambridge TechnologyCentre; the Jenkins Award to A. Lawley ofDrexel University; the Kroll Medal & Prizeto K.C. Mills of the National PhysicalLaboratory; the Nelton Award to R.J.Crawford of Queens' University; the Prain

Medal & Prize (sponsored by the CopperDevelopment Association) to W.S. Lyman,consultant; the Rosenhain Medal & Prizeto P. Gregson of Southampton University;the Stokowiec Medal & Prize to P. Beckleyof European Electrical Steels Ltd.; theThomas Medal & Prize to CM. Sellars ofthe University of Sheffield; the VerulamMedal & Prize to R.C. Hudd of BritishSteel Strip Products; the Williams Prize toS.G. Thornton of British Steel Teeside andF. Haers of Sidmar NV; the VanadiumAward (sponsored by VANTTEC) to W.B.Morrison of British Steel; the CharlesHatchett Award 1996 (sponsored byNiobium Products Company GmbH) toG.I. Rees of TWI, J. Perdix of Sollac, T.Maurickx of Sollac, H.K.D. Bhadeshia ofCambridge University, and C. Fossaert ofSollac; the A.T. Green Award to R.Damani of the University of Surrey; andthe T.B. Marsden Award to B.D. Gibsonof the Institute of Materials.

From the National Lecture Competition,

first prize went to Jacqueline Butterfieldof British Steel, second prize went to RuthWithey of the University of Birmingham,and third prize went to John Pugh of theUniversity of Strathclyde.

Further information on the prizes andthe 1996 recipients is available fromCarolyn Shaw, Awards Administrator,The Institute of Materials, 1 CarltonHouse Terrace, London SW1Y 5DB; 44-171-839-4071; fax 44-171-839-2071.

SBIR UpdateAdvanced Refractory Technology,

Inc. (Buffalo, New York) was award-ed $69,000 by the Naval SurfaceWarfare Center for evaluation of A1Nseparators in high-temperature batter-ies for underwater vehicle propulsion,as used for underwater unmannedvehicles (UUV).

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Oxyanions PromoteCrystallization of Zeolites

Researchers from the National ChemicalLaboratory in India reported in the May 23issue of Nature various "promoter" ionsthat speed up the crystallization rate of zeo-lites. With the addition of oxyanions (ClQr,PO43-, NOy, SO4

2-, CO32-, AsO43-, CIO3-,

B1O3", and IO3) to the molar gel composi-tion, the crystallization process of a range ofzeolite structures (NU-1, FER, MFI, ZSM-48, MTW, and BEA) accelerated. Theresearchers used fumed silica as a silicasource, stirred with template species, suchas quaternary ammonium ions, and alkaliin deionized water for one hour. Then thesolution of an aluminum source (NaAlO2 oraluminum sulf ate) was stirred into the sili-ca. The promoter was then stirred into thegel for one hour at room temperature,enhancing the crystallization process. At acrystallization temperature of 140cC forBEA, the crystallization process took nearly200 h crystallization time with no promoteras compared to under 50 h with the pro-moters perchlorate and phosphate and a lit-tle over 50 h with arsenate. According to theresearchers, "promoter oxyanions greatlypolarizes the hydrophobic hydrationspheres formed around silicate units andthe alkyl groups of the organic structure-directing agent, thereby facilitating theoverlapping of TPA-enclathrated silicatepolyanions. Such overlapping, in turn,forms the composite species at the onset ofcrystallization." The researchers reported acorrelation between the Z/r (charge/radiusratio) of the central cation of promoteroxyanions and the corresponding crystal-lization time of ZSM-5 synthesized with thepromoters. As the polarizing ability of theoxyanions increases, the crystallization rateincreases. The scientists concluded thationic species with greater polarizing abilityenhances the process of crystallization byaccelerating the condensation process.

Plasma Technology DestroysOrganic Contaminants in Soiland Ground Water

Los Alamos National Laboratory scien-tists have demonstrated a system thatdestroys volatile organic compounds(VOCs) found in ground water and soil.Using a nonthermal plasma that createshighly reactive molecules (free radicals)to break down the contaminants, the tech-nique has been used to extract VOCsfrom soil at McClellan Air Force Base,California, and from ground water atTinker Air Force Base, Oklahoma. Theplasma technology is likened to cold com-bustion; instead of using heat to break upcontaminants, plasma destroys molecules

using atoms or molecules that haveunpaired electrons.

At McClellan, the contaminants includebenzene, tolulene, acetone, freon, xylene,trichloroethelyne, trichloroethane, andperchloroethylene, some of which react inthe atmosphere and contribute to thedepletion of high-altitude ozone, the for-mation of ground-level ozone and, to alesser extent, acid rain. The plasma tech-nology treated a maximum of 10 ftVminof air and operated for 300 hours over atwo-month period. Researchers moni-tored gas flow, temperature, pressure,and electrical power.

At Tinker Air Force Base, ground waterwas pumped through an air stripper thatcascades the water within the strippingtower causing the volatile contaminantsto become airborne. Researchers pumpedthe air that came off the water stripperthrough the plasma, where it was treated.Clean air exited the system, while the left-over, less-hazardous compounds wererecovered in small, stainless steel tanksthat contained a dry scrubber material.

The plasma system consists of a 20-foottrailer filled with specialized equipment.The chemical reactions occur in an alu-minum tank that houses 20 nonthermalplasma cells. The nonthermal plasma cellsuse high-voltage electrical energy to cre-ate large quantities of highly reactive freeradicals. The free radicals subsequentlyreact with and break up hazardousorganic chemicals, converting them tononhazardous substances such as carbondioxide, water, and acids that can be neu-tralized. Most of the free radicals are oxy-gen atoms and hydroxyl molecules thatreact with and oxidize the larger mole-cules, thereby functioning much the sameas incineration, but without the heat andadded fuel exhaust.

Multiple Laser Reflections ofStress Monitoring ImproveElectronic, Magnetic, OpticalDevices in Noisy Environments

Scientists at Sandia National Labora-tories have developed a method to deter-mine stresses in very thin films of materialsused in advanced electronic, optical, andmagnetic devices. By beaming a one-halfmilliwatt laser into an angled, partiallyreflective mirror coated on both sides, anetalon (here, not used as an interferometer),researchers Eric Chason and Jerry Florocreate a series of internal reflections whichemerge as parallel beams of light. Thebeams are directed into the process cham-ber and onto the material surface over aregion of about one centimeter. The spac-ing between reflections of the beams are

monitored electronically using a videocamera. Distortions in the material as smallas one-hundredth of a micron can be mea-sured by the change in distance betweenthe reflected beams. The changing distancebecomes a continuous measure of warpageand thus, stress. To calibrate the amount ofstress in thin films, Chason and Floro mon-itor the curvature of the supporting materi-al to determine its warp while varying thetemperature or thickness of the film.

Instrument vibration never appears inthe readings because the rigid connectionbetween laser and etalon causes all thebeams to move together. This methodenables researchers to measure stress as itbuilds in a noisy environment rather thaninterrupt the process to remove the prod-uct for off-line analysis.

In a further improvement, the researchershave placed a second etalon rotated at rightangles to the first. This piggyback arrange-ment creates a square array of beams fromthe single source, making possible simulta-neous measurement over a square arearather than just along a line, and allowinganalysis of complex shapes.

Liquid Carbon Dioxide CleansUp Dry Cleaning

A system, developed under a collabo-ration between Los Alamos and HughesAircraft, replaces hazardous dry cleaningchemicals with a liquid carbon dioxidecleaning process. Under 800 to 1,000 psi,carbon dioxide acts like a liquid andserves as an organic, entirely recyclablesolvent that extracts dirt from clothing.When the liquid carbon dioxide isallowed to return to its gas state, dirt justfalls out. Repressurized, the carbon diox-ide can be used again. This process gener-ates no waste, other than the dirt.

According to Craig Taylor, principalinvestigator on the project in Los AlamosNational Laboratory, carbon dioxide dis-solves sweat, oils, and dirt.

The primary solvent used for manyyears by dry cleaners is perchloroethylene,or PERC, which is classified as a hazardoustoxic substance and is strictly regulatedunder the Clean Air Act and the Compre-hensive Environmental Response, Com-pensation and Liability Act. The liquid car-bon dioxide system will clean any materialthat is currently dry cleaned, and, in addi-tion, clean furs, leathers, and sequins.

ONR Honors Padture withYoung Investigator Award

Nitin P. Padture, an assistant professorin the Department of Metallurgy andMaterials Engineering at the University ofConnecticut, Storrs, has received a Young



Investigator Award from the Office ofNaval Research (ONR) for "exceptionalpromise for doing creative research andteaching." This award carries with it athree-year, $300,000 research grant, whichPadture will use for studying mechanicalbehavior of in sifu-reinforced ceramics.

Padture received his PhD degree fromLehigh University and has spent threeyears at the National Institute of Scienceand Technology as a postdoctoral fellowbefore joining the University of Connecticutfaculty in January 1995. His research inter-ests include processing and mechanicalbehavior of ceramics. He has published 27papers and is an advisor to the MaterialsResearch Society student chapter at theUniversity of Connecticut.

"Fuller Named Editor-in-Chief ofJournal of Electroceramics

Harry L. Tuller has been named theEditor-in-Chief of the newly formedKluwer Journal of Electroceramics. AsSumitomo Electric Industries Professor ofCeramics and Electronic Materials andDirector of the Crystal Physics andElectroceramics Laborary at the Massa-chusetts Institute of Technology, Tuller isknown for his research in solid-state ion-ics, grain-boundary-controlled semicon-ducting devices, defect theory, opticalproperties, sensor materials development,and semiconductor micromachining. Thejournal's editorial board comprises 29internationally known scientists with spe-cializations in the fields of electro-optics;ferro-, piezo-, and pyro-electrics; magnet-ic ceramics; processing/microstructuredevelopment; semiconductors/dielec-trics; sensors; and solid-state ionics.

1997 National Medal ofTechnology Call for Applications

The National Medal of Technology isthe highest honor awarded by thePresident of the United States for techno-logical innovation. Since 1985, the Medalhas annually been bestowed upon indi-viduals, teams, or companies for accom-plishments in the innovation, develop-ment, and commercialization of technolo-gy as evidenced by the establishment ofnew or significantly improved products,processes, or services.

The purpose of the program is to createan environment that fosters technologicalinnovation and recognizes the significantcontributions the U.S. leading innovatorshave made to the country's economicstrength and standard of living.

Nomination application packets for1997 can be obtained from the U.S. De-partment of Commerce by contacting theNational Medal of Technology Program

Director, Technology Administration,Room 4814C, U.S. Department ofCommerce, 14th Street and ConstitutionAvenue, NW, Washington, DC 20230;202-482-5572; fax 202-482-4817; [email protected]. gov; or theworld wide web http://www.ta.doc.gov/nmthome/nmt.htm.

The deadline for submission isSeptember 27,1996.

SARIS Analyzes SurfaceStructure and ChemicalReactions

Wayne Rabalais, chemistry professor atthe University of Houston, and two of hisgraduate students have developed a crys-tallography technique called scattering andrecoiling imaging spectrometry (SARIS) formonitoring surface structure and chemicalreactions on surfaces. By capturing imagesof ions in flight, Rabalais and his team areable to follow chemical reactions at a sur-face in real time. Using a large area, positionsensitive microchannel plate detector whichis gated so it can accept data only in smalltime windows—as short as 10 ns—Rabalaisand his team are gathering informationabout changes on the surface. Images show-ing spacial distribution of scattered particlesare collected digitally, then compared. Thisenables the researchers to determine wherea molecule reacts on a surface and how theatomic structure of the surface changes as aresult of the chemical reaction.

Rabalais and his team use a custom-made chamber that includes a 75 mm x 95mm detector plate surrounded by a vacu-um chamber. The chamber needs to beunusually large and oddly-shaped so thedetector could be moved through widearcs inside it.

Now beginning the third year on thisproject funded by the National ScienceFoundation, Rabalais is producing color-ful and artistic looking images of surfaces.

Cottrell Scholars to Receive$50,000 Research and TeachingAwards

Eighteen young faculty scientistsembarking on research and teachingcareers are the 1996 recipients of $50,000Cottrell Scholars Awards, which wereannounced by Research Corporation, afoundation for the advancement of sci-ence. The awards require no fixed bud-gets, permitting recipients to apply fundsas they think best to meet research andteaching objectives. Among the recipientsare George Nicholas Gibson, Universityof Connecticut: "Ultrafast Time-ResolvedMeasurements of the Ionization andDissociation of Molecules by Strong Laser

Fields"; David Howard Reitze, Universityof Florida: "Coherent Control of ChargeCarrier Motion in Semiconductor Hetero-structures"; Xiaoyang Zhu, SouthernIllinois University: "Surface ReactionDynamics in Chemical Vapor Deposi-tion"; David Z. Besson, University ofKansas: "Measurement of Coherent RadioWave Emission Induced by UltrahighEnergy Neutrino Interactions"; ZiqiangWang, Boston University, "CoulombInteraction, and Electronic Transport inHigh Magnetic Fields"; Mark ThomasTuominen, University of Massachusetts:"Measurements of Single-Electron Nano-structures in a Quantum Cavity: Manipu-lating the Quantum Interaction of Matterand Light"; Grover A. Swartzlander, Jr.,Worcester Polytechnic Institute: "Experi-mental Investigation of Optical SolitonsUsed as 'Optical Tweezers'"; Karl ToddMueller, The Pennsylvania State Univer-sity: "Efficient NMR Methods for Deter-mining Multiple Internuclear Distances inComplex Solids"; Mark Lee, University ofVirginia: "New Physics From an OldMaterial: Exploring the Correlated Motionof Interacting Electrons in Silicon"; BrianMax Tissue, Virginia Polytechnic Instituteand State University: "Characterization ofInterfaces in Nanocrystalline MaterialsUsing Laser Spectroscopy of LanthanideProbe Ions."

The Cottrell Scholars Awards are namedafter Frederick Gardner Cottrell, the scien-tist, inventor, and philanthropist whoestablished Research Corporation, a sci-ence advancement foundation, in 1912.The goals of the foundation are to makeinventions "more available and effective inthe useful arts" and "to provide means forscientific research and experimentation."

Charge Density WaveObserved on Lead-CoatedSurface of Ge Crystal

Researchers at the University of Tennes-see and Sandia National Laboratorieshave observed a charge density wave(CDW) localized at the lead-coated (111)surface of a germanium crystal. While atroom temperature a thin film of lead-coat-ed germanium appears to be metallic witha surface unit cell containing one Pb atomand three outer layer Ge atoms, each withan unpaired electron, at -20°C, a gradualand reversible electronic transition occurs.A small bandgap develops as the temper-ature decreases, resulting in a honeycombpattern charge arrangement. Theresearchers report in the May 30 issue ofNature, "On decreasing temperature, thePb/Ge(lll)-a system forms a commensu-rate surface charge density wave (SCDW)independent of any bulk phenomena."

8 MRS BULLETIN/AUGUST 1996


According to their report, the researchersused low-energy electron diffraction toascertain the symmetry of the surfaceatomic lattice, electron energy-loss spec-troscopy (EELS) to probe the excitationspectra of the interface, and scanning tun-neling microscopy to view the spatialvariations in the surface charge densitywith atomic resolution. One main incon-sistency they observed was, at low tem-perature, the unit cell contains three Pband nine Ge atoms, and 21 valence elec-trons. This finding contradicted the EELSobservation.

Microchip Thermocapillary PumpDrives Analysis of DNA

In an article published in the May 28issue of the Proceedings of the NationalAcademy of Sciences, David T. Burke, anassistant professor of human genetics at theUniversity of Michigan, and his colleaguesreported initial test results on five microfab-ricated components and their preliminaryintegration into a DNA-analyzing chip thatis 3 cm long and 0.5 cm wide.

"The heart of the device is a thermocapil-lary pump which uses surface tension ratherthan valves or moving parts, to mix drops ofpure DNA with an enzyme solution anddrive the DNA through five different com-ponents on the microchip," said Mark A.Burns, associate professor of chemical engi-neering at the University of Michigan.

The DNA solution forms discrete dropswith curved surfaces inside a series of nar-row channels on the device. Using micro-scopic heaters built into the chip, theresearchers heat one side of a drop whichreduces the surface tension and increasesthe internal pressure on that side. The pres-sure difference pushes the drop throughthe channel toward the direction of lowerpressure.

Researchers have moved samplesthrough all five processing steps on onesubstrate to produce DNA separations,which were visible through a microscope,according to Burns.

According to Burke, the current analysistechnique for DNA involves a time-con-suming process in which sequencing geneswith polymerase chain reaction requires amolecular biology laboratory and at least 10individual procedures. He said, "Our goalis to automate the process by shrinking thelab to fit on one silicon microchip."

Technical problems related to handlingsuch small amounts of liquid, and interac-tions between liquids and materials in the

chip remain to be solved. Work is current-ly underway to reduce the size of themicrochip to about one square centimeter.

This silicon wafer contains three of five compo-nents fabricated for use in one integratedmicrochip for DNA analysis. Individual com-ponents in the microchip include entry ports,transport channels, a thermally controlledreactor where mixing and enzyme digestion orpolymerase chain reaction amplificationoccurs, an electrophoresis channel, and adetector.

The square sections shown on the siliconwafer are microscopic heaters which drive thethermocapillary pumping function of thedevice, long, rectangular structures aremicron-sized channels for measuring, mixing,and moving tiny drops of DNA.

Be Atom Illustrates"Schrodinger's Cat" bySuperposition of Two States

When a team of physicists at theNational Institute of Standards and Tech-nology supercooled a beryllium atom witha laser, then hit it with five sequential puls-es of Raman beams, they caused the atomto oscillate, appearing in two positions atonce, that is, two coherent-state wave pack-ets. According to the physicists' report inthe May 24 issue of Science, the series oflaser pulses entangled the internal (elec-tronic) and external (motional) states of theion, creating a mesoscopic "Schrodinger'scat" state. The wave packets were separat-ed by a mesoscopic distance of more than80 nm.

The researchers said that each wavepacket is correlated with a particular inter-nal state of the atom. They applied anotherlaser pulse to couple the internal statesthen measured the interference of the dis-tinct wave packets. They reported, that thedifference frequency of the carrier Ramanbeams was set near aym/2n ~ 1.250 GHz

and the difference frequency of the dis-placement Raman beams was set to a^/ln= 11.2 MHz, which excited the motion ofthe ion to a coherent state from an initialzero-point state of motion in the harmonicpotential. The displacement force suppliesquantum entanglement of the internalstate with the external motional state. Thephysicists described the occurrence of theSchrodinger's cat state in five steps: theoriginal wave packet correlates to thequantum ground state of motion afterlaser-cooling; the wave packet is split afterapplication of the carrier beam; the initialinternal state wave packet is excited to acoherent state by the displacement beamforce, entangling the internal and motionalsystems; two distinct internal electronicquantum states of the atom exchangewave packets following another applica-tion of the carrier beam; then one of theinternal state's wave packets is excited to acoherent state by the displacement beamforce, causing the state of the atom to cor-respond most closely to that ofSchrodinger's cat.

Day Receives UMR's 1996Presidential Award

Delbert Day, Curators' Professor ofCeramic Engineering at the University ofMissouri—Rolla (UMR), has received theUniversity of Missouri System's 1996Presidential Award for Research andCreativity. The award, which includes a$15,000 stipend for research, is intended torecognize a UM faculty member for a sus-tained record of nationally and internation-ally prominent research or creativity.

Day is internationally recognized for hiswork on the structure and properties ofinorganic glasses. He conceived, alongwith Gary Ehrhardt of UM—Columbia,the idea of using glass microspheres toirradiate malignant tumors. The therapy,which is currently undergoing trials forpatients with kidney cancer, results inincreased life expectancy with none of thediscomforting side effects associated withradiation or chemotherapy. Day is also co-inventor of "glasphalt," a road-pavingsubstance that includes waste glass. Heholds 35 patents dealing with glassmicrospheres, ceramic dental materials,refractories, oxynitride glasses, and trans-parent composites.

Day earned his PhD degree in 1961 fromThe Pennsylvania State University andjoined the UMR faculty in 1961. •

1996 MRS Publications Catalog Supplement is available at 412-367-3003


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Denton Discovery™ 18