Liquid-phase deposition (LPD) from aqueous solution, under mild conditions of temperature (e55 °C) and pH (2.88-3.88), can produce thin (0.1-1.0 µm), adherent titania (TiO 2 ) films. This paper reports a systematic study of LPD TiO 2 films on variously prepared silicon wafer substrates, including (to our knowledge for the first time with LPD) several types of sulfonated surfaces (including sulfonated self-assembled monolayers and sulfonated polyelectrolyte multilayers). The growth rate and crystallinity of these films could be controlled by careful manipulation of solution parameters and surface functionality of the substrate.

Optical fluorescence sol-gel sensors have been developed for the detection of carbon dioxide gas in the 0.03-30% range with a detection limit of 0.008% (or 80 ppm) and a quantitation limit of 0.02% (or 200 ppm) CO(2). Sol-gels were spin-coated on glass slides to create an organically modified silica-doped matrix with the 1-hydroxypyrene-3,6,8-trisulfonate (HPTS) fluorescent indicator. The luminescence intensity of the HPTS indicator (513 nm) is quenched by CO(2), which protonates the anionic form of HPTS. An ion pair technique was used to incorporate the lipophilic dye into the hydrophilic sol-gel matrix. TiO(2) particles (<5 microm diameter) were added to induce Mie scattering and increase the incident light interaction with the sensing film, thus increasing the signal-to-noise ratio. Moisture-proof overcoatings have been used to maintain a constant level of water inside the sensor films. The optical sensors are inexpensive to prepare and can be easily coupled to fiber optics for remote sensing capabilities. A fiber-optic bundle was used for the gas detection and shown to work as part of a multianalyte platform for simultaneous detection of multiple analytes. The studies reported here resulted in the development of sol-gel optical fluorescent sensors for CO(2) gas with sensitivity below that in the atmosphere (ca. 387 ppm). These sensors are a complementary approach to current FT-IR measurements for real-time carbon dioxide detection in environmental applications.

The formation, degree of crystallinity, and adherence of dense titania (TiO 2 ) thin film coatings on a high-temperature polyimide resin (PMR-15) can be influenced by the chemical composition of the polymer surface. Furthermore, solution deposition conditions can be adjusted to provide additional control over the morphology and crystallinity of the titania films. Recipes for solution-based titania deposition that used a slowly hydrolyzing titanium fluoride salt in the presence of boric acid as a fluoride scavenger allowed growth of films up to 750 nm thick in 22 h. By adjusting solution pH and temperature, either amorphous titania or oriented crystalline anatase films could be formed. Surface sulfonate groups enhance the adhesion of solution-deposited oxide thin film coatings. While most sulfonation procedures severely damaged the PMR-15 surface, the use of chlorosulfonic acid followed by hydrolysis of the installed chlorosulfonyl groups provided effective surface sulfonation without significant surface damage. In some cases, the oxide deposition solution caused partial hydrolysis of the polymer surface, which itself was sufficient to allow adhesion of the titania film through chelation of titanium ions by exposed benzoic acid groups on the polymer surface.

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The pyrolysis of siloxy-anchored, organic self-assembled monolayers (SAMs) on oxide substrates [titanium dioxide powder; hydrolyzed silicon dioxide on (100) silicon] was studied using x-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and mass spectroscopy (MS). Pyrolysis in air began on heating at 200 °C and was complete by 400 °C for both octadecyltrichlorosilane (OTS) and C16-thioacetate (TA) SAMs, as observed in TGA of SAM-coated TiO2 powders, and in XPS studies of TA-SAM-coated TiO2 powders and Si wafers after various heat treatments. In low-oxygen environments, pyrolysis of SAMs began at higher temperatures: between 250 and 400 °C for heating in ultrahigh vacuum (10−8 Torr) as observed in XPS studies of TA-SAMs on Si, and between 300 and 400 °C in nitrogen, as observed in TEM analysis of sulfonate SAMs under a TiO2 thin film on Si substrates.

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Conventional fluorescence tomography provides images of the distribution of fluorescent agents within highly scattering media, but suffers from poor spatial resolution. Previously, we introduced a new method termed “temperature-modulated fluorescence tomography” (TM-FT) that generates fluorescence images with high spatial resolution. TM-FT first uses focused ultrasound to locate the distribution of temperature-sensitive fluorescence probes. Afterward, this a priori information is utilized to improve the performance of the inverse solver for conventional fluorescence tomography and reveal quantitatively accurate fluorophore concentration maps. However, the disadvantage of this novel method is the long data acquisition time as the ultrasound beam was scanned in a step-and-shoot mode. In this Letter, we present a new, fast scanning method that reduces the imaging time 40 fold. By continuously scanning the ultrasound beam over a 50 mm by 25 mm field-of-view, high-resolution fluorescence images are obtained in less than 29 min, which is critical for in vivo small animal imaging.