Use of information on the manufacture of samples for the optical characterization of multilayers through a global optimization

We present a procedure for the optical characterization of thin-film stacks from spectrophotometric data. The procedure overcomes the intrinsic limitations arising in the numerical determination of manyparameters from reflectance or transmittance spectra measurements. The key point is to use all theinformation available from the manufacturing process in a single global optimization process. The method is illustrated by a case study of solgel applications.

In situ fast ellipsometric analysis of repetitive surface phenomena

We present an ellipsometric technique and ellipsometric analysis of repetitive phenomena, based on the experimental arrangement of conventional phase modulated ellipsometers (PME) c onceived to study fast surface phenomena in repetitive processes such as periodic and triggered experiments. Phase modulated ellipsometry is a highly sensitive surface characterization technique that is widely used in the real-time study of several processes such as thin film deposition and etching. However, fast transient phenomena cannot be analyzed with this technique because precision requirements limit the data acquisition rate to about 25 Hz. The presented new ellipsometric method allows the study of fast transient phenomena in repetitive processes with a time resolution that is mainly limited by the data acquisition system. As an example, we apply this new method to the study of surface changes during plasma enhanced chemical vapor deposition of amorphous silicon in a modulated radio frequency discharge of SiH4. This study has revealed the evolution of the optical parameters of the film on the millisecond scale during the plasma on and off periods. The presented ellipsometric method extends the capabilities of PME arrangements and permits the analysis of fast surface phenomena that conventional PME cannot achieve.

Polyimide/SU-8 catheter-tip MEMS gauge pressure sensor.

This paper describes the development of a polyimide/SU-8 catheter-tip MEMS gauge pressure sensor. Finite element analysis was used to investigate critical parameters, impacting on the device design and sensing characteristics. The sensing element of the device was fabricated by polyimide-based micromachining on a flexible membrane, using embedded thin-film metallic wires as piezoresistive elements. A chamber containing this flexible membrane was sealed using an adapted SU-8 bonding technique. The device was evaluated experimentally and its overall performance compared with a commercial silicon-based pressure sensor. Furthermore, the device use was demonstrated by measuring blood pressure and heart rate in vivo.

Self-organizing propagation patterns from dynamic self-assembly in monolayers

Propagation of localized orientational waves, as imaged by Brewster angle microscopy, is induced by low intensity linearly polarized light inside axisymmetric smectic-C confined domains in a photosensitive molecular thin film at the air/water interface (Langmuir monolayer). Results from numerical simulations of a model that couples photoreorientational effects and long-range elastic forces are presented. Differences are stressed between our scenario and the paradigmatic wave phenomena in excitable chemical media.

Self-organizing propagation patterns from dynamic self-assembly in monolayers

Propagation of localized orientational waves, as imaged by Brewster angle microscopy, is induced by low intensity linearly polarized light inside axisymmetric smectic-C confined domains in a photosensitive molecular thin film at the air/water interface (Langmuir monolayer). Results from numerical simulations of a model that couples photoreorientational effects and long-range elastic forces are presented. Differences are stressed between our scenario and the paradigmatic wave phenomena in excitable chemical media.

Beneficial Effects of Selected Additives on Asphalt Cement Mixes, HR-278, 1987

Effects of polyolefins, neoprene, styrene-butadiene-styrene (SBS) block copolymers, styrene-butadiene rubber (SBR) latex, and hydrated lime on two asphalt cements were evaluated. Physical and chemical tests were performed on a total of 16 binder blends. Asphalt concrete mixes were prepared and tested with these modified binders and two aggregates (crushed limestone and gravel), each at three asphalt content levels. Properties evaluated on the modified binders (original and thin-film oven aged) included: viscosity at 25 deg C, 60 deg C and 135 deg C with capillary tube and cone-plate viscometer, penetration at 5 deg C and 25 deg C, softening point, force ductility, and elastic recovery at 10 deg C, dropping ball test, tensile strength, and toughness and tenacity tests at 25 deg C. From these the penetration index, the viscosity-temperature susceptibility, the penetration-viscosity number, the critical low-temperature, long loading-time stiffness, and the cracking temperature were calculated. In addition, the binders were studied with x-ray diffraction, reflected fluorescence microscopy, and high-performance liquid chromatography techniques. Engineering properties evaluated on the 72 asphalt concrete mixes containing additives included: Marshall stability and flow, Marshall stiffness, voids properties, resilient modulus, indirect tensile strength, permanent deformation (creep), and effects of moisture by vacuum-saturation and Lottman treatments. Pavement sections of varied asphalt concrete thicknesses and containing different additives were compared to control mixes in terms of structural responses and pavement lives for different subgrades. Although all of the additives tested improved at least one aspect of the binder/mixture properties, no additive was found to improve all the relevant binder/mixture properties at the same time. On the basis of overall considerations, the optimum beneficial effects can be expected when the additives are used in conjunction with softer grade asphalts.

Behavior of Asphalts During Production of Asphaltic Concrete Mixes, HR-107, 1965

When mixing asphalt in thin film and at high temperatures, as in the production of asphalt concrete, it has been shown that asphalt will harden due essentially to two factors: (1) losses of volatiles and (2) oxidation. The degree of hardening as expressed by percent loss in penetration varied from as low as 7% to about 57% depending on mixing temperatures, aggregate types, gradation, asphalt content, penetration and other characteristics of asphalts used. Methods used to predict hardening during mixing include loss on heat and thin film oven tests, with the latter showing better correlation with the field findings. However, information on other physical and chemical changes that may occur as a result of mixing in the production of hot-mix asphaltic concrete is limited, The purpose of this research project was to ascertain the changes of asphalt cement properties, both physical and chemical, during mixing operation and to determine whether one or more of the several tests of asphalt cements were critical enough to indicate these changes.

Determination of Asphalt Content and Characteristics of Bituminous Paving Mixtures, MLR-88-11, 1988

Due to the hazardous nature of chemical asphalt extraction agents, nuclear gauges have become an increasingly popular method of determining the asphalt content of a bituminous mix. This report details the results of comparisons made between intended, tank stick, extracted, and nuclear asphalt content determinations. A total of 315 sets of comparisons were made on samples that represented 110 individual mix designs and 99 paving projects. All samples were taken from 1987 construction projects. In addition to the comparisons made, seventeen asphalt cement samples were recovered for determination of penetration and viscosity. Results were compared to similar tests performed on the asphalt assurance samples in an attempt to determine the amount of asphalt hardening that can be expected due to the hot mix process. Conclusions of the report are: 1. Compared to the reflux extraction procedure, nuclear asphalt content gauges determine asphalt content of bituminous mixes with much greater accuracy and comparable precision. 2. As a means for determining asphalt content, the nuclear procedure should be used as an alternate to chemical extractions whenever possible. 3. Based on penetration and viscosity results, softer grade asphalts undergo a greater degree 'of hardening due to hot mix processing than do harder grades, and asphalt viscosity changes caused by the mixing process are subject to much more variability than are changes in penetration. 4. Based on changes in penetration and viscosity, the Thin Film Oven Test provides a reasonable means of estimating how much asphalt hardening can be anticipated due to exposure to the hot mix processing environment.

Selective ablation of photovoltaic materials with UV laser sources for monolithic interconnection of devices based on a-Si:H

Lasers are essential tools for cell isolation and monolithic interconnection in thin-film-silicon photovoltaic technologies. Laser ablation of transparent conductive oxides (TCOs), amorphous silicon structures and back contact removal are standard processes in industry for monolithic device interconnection. However, material ablation with minimum debris and small heat affected zone is one of the main difficulty is to achieve, to reduce costs and to improve device efficiency. In this paper we present recent results in laser ablation of photovoltaic materials using excimer and UV wavelengths of diode-pumped solid-state (DPSS) laser sources. We discuss results concerning UV ablation of different TCO and thin-film silicon (a-Si:H and nc-Si:H), focussing our study on ablation threshold measurements and process-quality assessment using advanced optical microscopy techniques. In that way we show the advantages of using UV wavelengths for minimizing the characteristic material thermal affection of laser irradiation in the ns regime at higher wavelengths. Additionally we include preliminary results of selective ablation of film on film structures irradiating from the film side (direct writing configuration) including the problem of selective ablation of ZnO films on a-Si:H layers. In that way we demonstrate the potential use of UV wavelengths of fully commercial laser sources as an alternative to standard backscribing process in device fabrication.

Bituminous Mixes Prepared with Foamed Asphalt, Iowa Highway Research Board Bulletin No. 18, 1960

A contract for Project HR-20 "Treating Loess, Fine Sands and Soft Limestones with Liquid Binders" of the Iowa Highway Research Board was awarded in December, 1951, to the Iowa Engineering Experiment Station of Iowa State University as its Project 295-S. By 1954 the studies of the fine materials and asphalts had progressed quite well, and a method of treating the fine materials, called the atomization process, had been applied. A study was begun in 1954 to see if some of the problems of the atomization process could be solved with the use of foamed asphalt. Foamed asphalt has several advantages. The foaming of asphalt increases its volume, reduces its viscosity, and alters its surface tension so that it will adhere tenaciously to solids. Foamed asphalt displaces moisture from the surface of a solid and coats it with a thin film. Foamed asphalt can permeate deeply into damp soils. In the past these unusual characteristics were considered nuisances to be avoided if possible.

Investigation ofsolid - state cooler based on electrocaloric effect

Electrocaloric cooling based on ability of material to change temperature by applying an electric field under adiabatic conditions is relatively new and challenging direction of ferroelectrics research. In this work we report about analytical, simulation and experimental data for BaSrTiO3 thin film and bulk ceramic samples. Detailed discussion of a theoretical base of the electrocaloric effect is included. Demonstrated experimental and computational results exemplify rational approach to a problem of solid-state cooler construction.

Väkevän urealiuoksen puhdistaminen kalvotekniikalla

Kirjallisuusosassa käsiteltiin nanosuodatus-, käänteisosmoosi- ja elektrodialyysitekniikoita liuosten puhdistuksessa. Nanosuodatuksella ja käänteisosmoosilla voidaan liuottimesta erottaa pienen moolimassan omaavia liuenneita aineita ohuen kalvon avulla. Nanosuodatuksessa ja käänteisosmoosissa ajavana voimana on paine, jonka tulee ylittää liuoksen osmoottinen paine. Elektrodialyysissä ajavana voimana toimii sähköpotentiaaliero. Tekniikka käyttää hyväkseen ionien tai molekyylien kykyä johtaa sähköä. Elektrodialyysillä voidaan liuoksesta erottaa toisistaan varauksettomat ja varaukselliset komponentit sähköä johtavan membraanin avulla. Kokeellisessa osassa väkevää ureavesiliuosta suodatettiin nanosuodatus- ja käänteisosmoosikalvoilla tutkien paineen, lämpötilan ja konsentroitumisen vaikutusta vuohonja retentioon. Tarkoituksena oli saada urea tuotteena permeaattiin ja epäpuhtaudet erottumaan retentaattiin. Permeaattien epäpuhtauksien pitoisuuksia verrattiin tuotteen spesifikaation raja-arvoihin. Suodatukset tehtiin Lappeenrannan teknillisen yliopiston tiloissa DSS Labstak M20 suotimella. Työssä käytettiin NF1-, NF2-, NF270-, NF-, NF90-, Desal-5 DK-, OPMN-P 70- ja TFC ULP-kalvoja. Nanosuodatuskalvot NF2- ja NF270 antoivat parhaan vuon ja erotuskyvyn suhteen puhdistettaessa urealiuosta. Paineen noustessa kalvojen retentiot paranivat. Lämpötilan noustessa vuo parani, joskin täytyy huomioida urean kiihtyvä hajoaminen lähestyttäessä 40 °C astetta. Kalvojen kestävyyttä ureasuodatuksissa ei voitu näiden kokeiden avulla varmentaa.

Cryo-electron microscopy of vitreous sections of native biological cells and tissues : methodology and applications

Résumé L'eau est souvent considérée comme une substance ordinaire puisque elle est très commune dans la nature. En fait elle est la plus remarquable de toutes les substances. Sans l'eau la vie sur la terre n'existerait pas. L'eau représente le composant majeur de la cellule vivante, formant typiquement 70 à 95% de la masse cellulaire et elle fournit un environnement à d'innombrables organismes puisque elle couvre 75% de la surface de terre. L'eau est une molécule simple faite de deux atomes d'hydrogène et un atome d'oxygène. Sa petite taille semble en contradiction avec la subtilité de ses propriétés physiques et chimiques. Parmi celles-là, le fait que, au point triple, l'eau liquide est plus dense que la glace est particulièrement remarquable. Malgré son importance particulière dans les sciences de la vie, l'eau est systématiquement éliminée des spécimens biologiques examinés par la microscopie électronique. La raison en est que le haut vide du microscope électronique exige que le spécimen biologique soit solide. Pendant 50 ans la science de la microscopie électronique a adressé ce problème résultant en ce moment en des nombreuses techniques de préparation dont l'usage est courrant. Typiquement ces techniques consistent à fixer l'échantillon (chimiquement ou par congélation), remplacer son contenu d'eau par un plastique doux qui est transformé à un bloc rigide par polymérisation. Le bloc du spécimen est coupé en sections minces (d’environ 50 nm) avec un ultramicrotome à température ambiante. En général, ces techniques introduisent plusieurs artefacts, principalement dû à l'enlèvement d'eau. Afin d'éviter ces artefacts, le spécimen peut être congelé, coupé et observé à basse température. Cependant, l'eau liquide cristallise lors de la congélation, résultant en une importante détérioration. Idéalement, l'eau liquide est solidifiée dans un état vitreux. La vitrification consiste à refroidir l'eau si rapidement que les cristaux de glace n'ont pas de temps de se former. Une percée a eu lieu quand la vitrification d'eau pure a été découverte expérimentalement. Cette découverte a ouvert la voie à la cryo-microscopie des suspensions biologiques en film mince vitrifié. Nous avons travaillé pour étendre la technique aux spécimens épais. Pour ce faire les échantillons biologiques doivent être vitrifiés, cryo-coupées en sections vitreuse et observées dans une cryo-microscope électronique. Cette technique, appelée la cryo- microscopie électronique des sections vitrifiées (CEMOVIS), est maintenant considérée comme étant la meilleure façon de conserver l'ultrastructure de tissus et cellules biologiques dans un état très proche de l'état natif. Récemment, cette technique est devenue une méthode pratique fournissant des résultats excellents. Elle a cependant, des limitations importantes, la plus importante d'entre elles est certainement dû aux artefacts de la coupe. Ces artefacts sont la conséquence de la nature du matériel vitreux et le fait que les sections vitreuses ne peuvent pas flotter sur un liquide comme c'est le cas pour les sections en plastique coupées à température ambiante. Le but de ce travail a été d'améliorer notre compréhension du processus de la coupe et des artefacts de la coupe. Nous avons ainsi trouvé des conditions optimales pour minimiser ou empêcher ces artefacts. Un modèle amélioré du processus de coupe et une redéfinitions des artefacts de coupe sont proposés. Les résultats obtenus sous ces conditions sont présentés et comparés aux résultats obtenus avec les méthodes conventionnelles. Abstract Water is often considered to be an ordinary substance since it is transparent, odourless, tasteless and it is very common in nature. As a matter of fact it can be argued that it is the most remarkable of all substances. Without water life on Earth would not exist. Water is the major component of cells, typically forming 70 to 95% of cellular mass and it provides an environment for innumerable organisms to live in, since it covers 75% of Earth surface. Water is a simple molecule made of two hydrogen atoms and one oxygen atom, H2O. The small size of the molecule stands in contrast with its unique physical and chemical properties. Among those the fact that, at the triple point, liquid water is denser than ice is especially remarkable. Despite its special importance in life science, water is systematically removed from biological specimens investigated by electron microscopy. This is because the high vacuum of the electron microscope requires that the biological specimen is observed in dry conditions. For 50 years the science of electron microscopy has addressed this problem resulting in numerous preparation techniques, presently in routine use. Typically these techniques consist in fixing the sample (chemically or by freezing), replacing its water by plastic which is transformed into rigid block by polymerisation. The block is then cut into thin sections (c. 50 nm) with an ultra-microtome at room temperature. Usually, these techniques introduce several artefacts, most of them due to water removal. In order to avoid these artefacts, the specimen can be frozen, cut and observed at low temperature. However, liquid water crystallizes into ice upon freezing, thus causing severe damage. Ideally, liquid water is solidified into a vitreous state. Vitrification consists in solidifying water so rapidly that ice crystals have no time to form. A breakthrough took place when vitrification of pure water was discovered. Since this discovery, the thin film vitrification method is used with success for the observation of biological suspensions of. small particles. Our work was to extend the method to bulk biological samples that have to be vitrified, cryosectioned into vitreous sections and observed in cryo-electron microscope. This technique is called cryo-electron microscopy of vitreous sections (CEMOVIS). It is now believed to be the best way to preserve the ultrastructure of biological tissues and cells very close to the native state for electron microscopic observation. Since recently, CEMOVIS has become a practical method achieving excellent results. It has, however, some sever limitations, the most important of them certainly being due to cutting artefacts. They are the consequence of the nature of vitreous material and the fact that vitreous sections cannot be floated on a liquid as is the case for plastic sections cut at room temperature. The aim of the present work has been to improve our understanding of the cutting process and of cutting artefacts, thus finding optimal conditions to minimise or prevent these artefacts. An improved model of the cutting process and redefinitions of cutting artefacts are proposed. Results obtained with CEMOVIS under these conditions are presented and compared with results obtained with conventional methods.

In situ spectroellipsometric study of the nucleation and growth of amorphous silicon

A detailed in situ spectroellipsometric analysis of the nucleation and growth of hydrogenated amorphous silicon (a:Si:H) is presented. Photoelectronic quality a‐Si:H films are deposited by plasma‐enhanced chemical vapor deposition on smooth metal (NiCr alloy) and crystalline silicon (c‐Si) substrates. The deposition of a‐Si:H is analyzed from the first monolayer up to a final thickness of 1.2 μm. In order to perform an improved analysis, real time ellipsometric trajectories are recorded, using fixed preparation conditions, at various photon energies ranging from 2.2 to 3.6 eV. The advantage of using such a spectroscopic experimental procedure is underlined. New insights into the nucleation and growth mechanisms of a‐Si:H are obtained. The nucleation mechanism on metal and c‐Si substrates is very accurately described assuming a columnar microstructural development during the early stage of the growth. Then, as a consequence of the incomplete coalescence of the initial nuclei, a surface roughness at the 10-15 Å scale is identified during the further growth of a‐Si:H on both substrates. The bulk a‐Si:H grows homogeneously beneath the surface roughness. Finally, an increase of the surface roughness is evidenced during the long term growth of a‐Si:H. However, the nature of the substrate influenced the film growth. In particular, the film thickness involved in the nucleation‐coalescence phase is found lower in the case of c‐Si (67±8 Å) as compared to NiCr (118±22 Å). Likewise films deposited on c‐Si present a smaller surface roughness even if thick samples are considered (>1 μm). More generally, the present study illustrates the capability of in situ spectroellipsometry to precisely analyze fundamental processes in thin‐film growth, but also to monitor the preparation of complex structures on a few monolayers scale.

Optoelectronic studies in nanocrystalline silicon Schottky diodes obtained by Hot-Wire Chemical Vapour Deposition

The very usual columnar growth of nanocrystalline silicon leads to electronic transport anisotropies. Whereas electrical measurements with coplanar electrodes only provide information about the electronic transport parallel to the substrate, it is the transverse transport which determines the collection efficiency in thin film solar cells. Hence, Schottky diodes on transparent electrodes were obtained by hot-wire CVD in order to perform external quantum efficiency and surface photovoltage studies in sandwich configuration. These measurements allowed to calculate a transverse collection length, which must correlate with the photovoltaic performance of thin film solar cells. Furthermore, the density of charge trapped at localized states in the bandgap was estimated from the voltage dependence of the depletion capacitance of these rectifying contacts.