Publications

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The lubrication of silicon surfaces with alcohol vapors has recently been demonstrated. With a sufficient concentration of pentanol vapor present, sliding of a silica ball on an oxidized silicon wafer can proceed with no measurable wear. The initial results of time-of-flight secondary ion mass spectrometry (ToF-SIMS) analysis of wear surfaces revealed a reaction product having thickness on the order of a monolayer, and with an ion spectrum that included fragments having molecular weights of 200 or more that occurred only inside the wear tracks. The parent alcohol molecule pentanol, has molecular weight of 88amu, suggesting that reactions of adsorbed alcohols on the wearing surfaces allowed polymerization of the alcohols to form higher molecular weight species. In addition to pin-on-disk studies, lubrication of silicon surfaces with pentanol vapors has also been demonstrated using MicroElectroMechanical Systems (MEMS) devices. Recent investigations of the reaction mechanisms of the alcohol molecules with the oxidized silicon surfaces have shown that wearless sliding requires a concentration of the alcohol vapor that is dependent upon the contact stress during sliding, with higher stress requiring a greater concentration of alcohol. Different vapor precursors including those with acid functionality, olefins, and methyl termination also produce polymeric reaction products, and can lubricate the silica surfaces. Doping the operating environment with oxygen was found to quench the formation of the polymeric reaction product, and demonstrates that polymer formation is not necessary for wearless sliding.

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An overwhelming majority of metamaterial designs that have been proposed thus far rely on the use of metallic resonators to afford properties that are unprecedented in nature. Though well suited for applications at radio and microwave frequencies, metals experience severe ohmic losses at higher frequencies rendering their use at such frequencies impractical. Certainly the future of metamaterials lies in their implementation in the visible and long wavelength infrared (LWIR, 8-12 {micro}m). Thus, alternative design protocols and material components tailored specifically for these frequencies are highly attractive. Herein, we present low permittivity, low permeability polymer dielectric materials that are well suited substrates for LWIR-metamaterial applications. These materials lack vibrational absorption bands in the 8-12 {micro}m range are 3D fabrication compatible, photopatternable, and high temperature tolerant. Thus, these materials are ideal for fabrication of 3D metamaterial structures operating in the LWIR and can also serve as negative photoresists for contact lithography applications.

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Materials with switchable states are desirable in many areas of science and technology. The ability to thermally transform a dielectric material to a conductive state should allow for the creation of electronics with built-in safety features. Specifically, the non-desirable build-up and discharge of electricity in the event of a fire or over-heating would be averted by utilizing thermo-switchable dielectrics in the capacitors of electrical devices (preventing the capacitors from charging at elevated temperatures). We have designed a series of polymers that effectively switch from a non-conductive to a conductive state. The thermal transition is governed by the stability of the leaving group after it leaves as a free entity. Here, we present the synthesis and characterization of a series of precursor polymers that eliminate to form poly(p-phenylene vinylene) (PPV's).

Materials with switchable states are desirable in many areas of science and technology. The ability to thermally transform a dielectric material to a conductive state should allow for the creation of electronics with built-in safety features. Specifically, the non-desirable build-up and discharge of electricity in the event of a fire or over-heating would be averted by utilizing thermo-switchable dielectrics in the capacitors of electrical devices (preventing the capacitors from charging at elevated temperatures). We have designed a series of polymers that effectively switch from a non-conductive to a conductive state. The thermal transition is governed by the stability of the leaving group after it leaves as a free entity. Here, we present the synthesis and characterization of a series of precursor polymers that eliminate to form poly(p-phenylene vinylene) (PPV's).

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A gradient array apparatus was constructed for the study of porous polymers produced using the process of chemically-induced phase separation (CIPS). The apparatus consisted of a 60 element, two-dimensional array in which a temperature gradient was placed in the y-direction and composition was varied in the x-direction. The apparatus allowed for changes in opacity of blends to be monitored as a function of temperature and cure time by taking images of the array with time. The apparatus was validated by dispense a single blend composition into all 60 wells of the array and curing them for 24 hours and doing the experiment in triplicate. Variations in micron scale phase separation were readily observed as a function of both curing time and temperature and there was very good well-to-well consistency as well as trial-to-trial consistency. Poragen of samples varying with respect to cure temperature was removed and SEM images were obtained. The results obtained showed that cure temperature had a dramatic affect on sample morphology, and combining data obtained from visual observations made during the curing process with SEM data can enable a much better understanding of the CIPS process and provide predictive capability through the relatively facile generation of composition-process-morphology relationships. Data quality could be greatly enhanced by making further improvements in the apparatus. The primary improvements contemplated include the use of a more uniform light source, an optical table, and a CCD camera with data analysis software. These improvements would enable quantification of the amount of scattered light generated from individual elements as a function of cure time. In addition to the gradient array development, porous composites were produced by incorporating metal particles into a blend of poragen, epoxy resin, and crosslinker. The variables involved in the experiment were metal particle composition, primary metal particle size, metal concentration, and poragen composition. A total of 16 different porous composites were produced and characterized using SEM. In general, the results showed that pore morphology and the distribution of metal particles was dependent on multiple factors. For example, the use of silver nanoparticles did not significantly affect pore morphology for composites derived from decanol as the poragen, but exceptionally large pores were obtained with the use of decane as the poragen. With regard to the effect of metal particle size, silver nanoparticles were essentially exclusively dispered in the polymer matrix while silver microparticles were found in pores. For nickel particles, both nanoparticles and microparticles were largely dispersed in the polymer matrix and not in the pores.

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This paper presents the development of a sensor to detect the oxidative and radiation induced degradation of polypropylene. Recently we have examined the use of crosslinked assemblies of nanoparticles as a chemiresistor-type sensor for the degradation products. We have developed a simple method that uses a siloxane matrix to fabricate a chemiresistor-type sensor that minimizes the swelling transduction mechanism while optimizing the change in dielectric response. These sensors were exposed with the use of a gas chromatography system to three previously identified polypropylene degradation products including 4-methyl-2-pentanone, acetone, and 2-pentanone. The limits of detection 210 ppb for 4-methy-2-pentanone, 575 ppb for 2-pentanone, and the LoD was unable to be determined for acetone due to incomplete separation from the carbon disulfide carrier.

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Both conventional and combinatorial approaches were used to study the pore formation process in epoxy based polymer systems. Sandia National Laboratories conducted the initial work and collaborated with North Dakota State University (NDSU) using a combinatorial research approach to produce a library of novel monomers and crosslinkers capable of forming porous polymers. The library was screened to determine the physical factors that control porosity, such as porogen loading, polymer-porogen interactions, and polymer crosslink density. We have identified the physical and chemical factors that control the average porosity, pore size, and pore size distribution within epoxy based systems.

Conductive polymers have become an extremely useful class of materials for many optical applications. We have developed an electrochemical growth method for depositing highly conductive ({approx}100 S/cm) polypyrrole. Additionally, we have adapted advanced fabrication methods for use with the polypyrrole resulting in gratings with submicron features. This conductive polymer micro-wire grid provides an optical polarizer with unique properties. When the polymer is exposed to ionizing radiation, its conductivity is affected and the polarization properties of the device, specifically the extinction ratio, change in a corresponding manner. This change in polarization properties can be determined by optically interrogating the device, possibly from a remote location. The result is a passive radiation-sensitive sensor with very low optical visibility. The ability to interrogate the device from a safe standoff distance provides a device useful in potentially dangerous environments. Also, the passive nature of the device make it applicable in applications where external power is not available. We will review the polymer deposition, fabrication methods and device design and modeling. The characterization of the polymer's sensitivity to ionizing radiation and optical testing of infrared polarizers before and after irradiation will also be presented. These experimental results will highlight the usefulness of the conductive infrared polarizer to many security and monitoring applications.

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Remote detection of radiation is a difficult problem due to the 1/r 2 fall-off Recent advances in polymer research and nanoscale fabrication methods along with advances in optical Polarimetrie remote sensing systems suggest a solution. The basic device uses a micro-wiregrid infrared polarizer fabricated in conductive polymer. When the polymer is exposed to hard radiation, its conductivity will be affected and the polarization properties of the device will change in a corresponding manner. This change in polarization properties can be determined by optically interrogating the device, possibly from a remote location. We will report on the development of a radiation-sensitive passive dosimeter polymer with very low optical visibility. Progress on material development, lithographic fabrication and optical characterization will be presented.

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