Stephen Semancik

Tin oxide gas sensor fabricated using CMOS micro-hotplates and in-situ processing

A monolithic tin oxide (SnO/sub 2/) gas sensor realized by commercial CMOS foundry fabrication (MOSIS) and postfabrication processing techniques is reported. The device is composed of a sensing film that is sputter-deposited on a silicon micromachined hotplate. The fabrication technique requires no masking and utilizes in situ process control and monitoring of film resistivity during film growth. Microhotplate temperature is controlled from ambient to 500 degrees C with a thermal efficiency of 8 degrees C/mW and thermal response time of 0.6 ms. Gas sensor responses of pure SnO/sub 2/ films to H/sub 2/ and O/sub 2/ with an operating temperature of 350 degrees C are reported. The fabrication methodology allows integration of an array of gas sensors of various films with separate temperature control for each element in the array, and circuits for a low-cost CMOS-based gas sensor system.<<ETX>>

Microhotplate Platforms for Chemical Sensor Research

Abstract This paper describes the development and use of microdevices and microarrays in chemical sensor research. The surface-micromachined “microhotplate” structure common within the various platforms included here was originally designed for fabricating conductometric gas microsensor prototypes. Microhotplate elements include functionality for measuring and controlling temperature, and measuring the electrical properties of deposited films. As their name implies, they are particularly well-suited for examining temperature-dependent phenomena on a micro-scale, and their rapid heating/cooling characteristics has led to the development of low power sensors that can be operated in dynamic temperature programmed modes. Tens or hundreds of the microhotplates can be integrated within arrays that serve as platforms for efficiently producing processing/performance correlations for sensor materials. The microdevices also provide a basis for developing new types of sensing prototypes and can be used in investigations of proximity effects and surface transient phenomena.

Selected-Area Deposition of Multiple Active Films for Conductometric Microsensor Arrays

Abstract A new generation of planar conductometric gas sensors is being developed which combines active semiconducting oxide films with Si-micromachined ‘micro-hotplate’ array structures. These devices are tailored for a variety of applications by tuning both the composition of multiple types of active films and the temperature cycles programmed for individual elements within an array. In this paper we described and demonstrate the approach, and present results for, a chemical vapor deposition (CVD)-based self-lithographic microfabrication method. This method is being examined as a highly efficient and compatible means of depositing oxide films and low-coverage catalytic metal overlayers on the microsensor elements of micro-hotplate arrays. Real-time monitoring of the film growth processe is provided by conductance measurements, and surveys of processing/property relationships can be performed in a very effective manner to determine optimal fabrication methods for multiple-active material arrays.

Thermal and sputtered aluminum oxide coatings for high temperature electrical insulation

Aluminum oxide coatings have been investigated as electrically insulating layers for mounting thin film Pt–Pt/Rh thermocouples on gas turbine blade and vane alloys (MAR M200 + Hf and MAR M509). Thermal oxides were grown directly onto NiCoCrAlY and FeCrAlY coatings on these alloys at temperature between 1300 and 1400 K in oxygen partial pressures 10−7 to 2×104 Pa. Although these thermal oxides exhibited good adherence, analytical characterizations using electron and optical microscopy, as well as x‐ray photoelectron spectroscopy (XPS) showed that they had defects and impurities which limited their insulating ability. The insulating quality of the coating was greatly improved however by reactively sputtering an aluminum oxide film over the thermal oxide. Results are presented on the electrical performance of the 2–5 μm thick composite layers for temperatures up to 1300 K.

Doping effects and reversibility studies on gas-exposed α-sexithiophene thin films

The electronic effects produced by controlled gas exposures on α-sexithiophene thin films have been investigated using x-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). Incremental exposures of α6T films to NO2, O2, NH3 in N2, and water vapor in N2 were performed in ultrahigh vacuum, while repeated doses of O2, H2 in N2, and methanol vapor in N2 were performed ex situ at ambient pressure. In both conditions XPS spectra of gas-exposed films showed no evidence of chemical changes. However, the features in both XPS and UPS spectra were observed to shift as a function of gas dosage, with the magnitude dependent on each particular gas. These effects could be reversed by heating the films to temperatures around 100 K. This behavior is interpreted in terms of doping by weakly bonded gas species within the near-surface region of the α6T films. Greater doping effects were observed for films dosed at ambient pressure. We discuss possible gas adsorption models that may explain ...

Multi-resonant plasmonic nanodome arrays for label-free biosensing applications

The characteristics and utility of plasmonic nanodome arrays capable of supporting multiple resonance modes are described. A low-cost, large-area replica molding process is used to produce, on flexible plastic substrates, two-dimensional periodic arrays of cylinders that are subsequently coated with SiO2 and Ag thin films to form dome-shaped structures, with 14 nm spacing between the features, in a precise and reproducible fashion. Three distinct optical resonance modes, a grating diffraction mode and two localized surface plasmon resonance (LSPR) modes, are observed experimentally and confirmed by finite-difference-time-domain (FDTD) modeling which is used to calculate the electromagnetic field distribution of each resonance around the nanodome array structure. Each optical mode is characterized by measuring sensitivity to bulk refractive index changes and to surface effects, which are examined using stacked polyelectrolyte layers. The utility of the plasmonic nanodome array as a functional interface for biosensing applications is demonstrated by performing a bioassay to measure the binding affinity constant between protein A and human immunoglobulin G (IgG) as a model system. The nanoreplica molding process presented in this work allows for simple, inexpensive, high-throughput fabrication of nanoscale plasmonic structures over a large surface area (120 × 120 mm(2)) without the requirement for high resolution lithography or additional processes such as etching or liftoff. The availability of multiple resonant modes, each with different optical properties, allows the nanodome array surface to address a wide range of biosensing problems with various target analytes of different sizes and configurations.

In situ conductivity characterization of oxide thin film growth phenomena on microhotplates

Through the use of silicon micromachining, we have developed a microhotplate structure capable of reaching temperatures in excess of 500 °C, onto which thin films have been selectively grown via metalorganic chemical vapor deposition. The microhotplate structure contains surface electrical contacts which permit conductance measurements to be made on films during and after deposition, and therefore presents some unique opportunities for the in situ characterization of growing films as well as for novel gas sensing approaches. We have investigated the deposition of conducting oxides such as SnO2 and ZnO on these microhotplate platforms for gas sensing applications. The conductance of the deposited films has been measured in situ as a function of time, and used in combination with postdeposition thickness measurements to provide insights into the growth rate of the oxide films. Results indicate that our conductance measurements are sensitive, in certain cases, to changes in the film thickness on the order of...

A monolithic implementation of interface circuitry for CMOS compatible gas-sensor system

A monolithic micro-gas-sensor system, designed and fabricated in a standard CMOS process, is described. The gas-sensor system incorporates an array of four microhotplate-based gas-sensing structures. The system utilizes a thin film of tin oxide (SnO/sub 2/) as a sensing material. The interface circuitry on the chip has digital decoders to select each element of the sensing array and an operational amplifier to monitor the change in conductance of the film. The chip is post-processed to create microhotplates using bulk micro-machining techniques. Measurements are presented for various portions of the interface circuitry used for the gas-sensor system.

Gas Sensing with Bare and Graphene-covered Optical Nano Antenna Structures

The motivation behind this work is to study the gas phase chemical sensing characteristics of optical (plasmonic) nano-antennas (ONA) and graphene/graphene oxide-covered versions of these structures. ONA are devices that have their resonating frequency in the visible range. The basic principle governing the detection mechanism for ONA is refractive index sensing. The change in the concentration of the analyte results in a differing amount of adsorbate and correlated shifts in the resonance wavelength of the device. In this work, bare and graphene or graphene oxide covered ONA have been evaluated for gas sensing performance. Four different analytes (ethanol, acetone, nitrogen dioxide and toluene) were used in testing. ONA response behavior to different analytes was modified by adsorption within the graphene and graphene oxide overlayers. This work is a preliminary study to understand resonance wavelength shift caused by different analytes. Results imply that the combination of well-structured ONA functionalized by graphene-based adsorbers can give sensitive and selective sensors but baseline drift effects identified in this work must be addressed for applied measurements.

Effect of interdome spacing on the resonance properties of plasmonic nanodome arrays for label-free optical sensing

In this paper, we report on experimental and theoretical studies that investigate how the structural properties of plasmonic nanodome array devices determine their optical properties and sensing performance. We examined the effect of the interdome gap spacing within the plasmonic array structures on the performance for detection of change in local refractive index environment for label-free capture affinity biosensing applications. Optical sensing properties were characterized for nanodome array devices with interdome spacings of 14 nm, 40 nm, and 79 nm, as well as for a device where adjacent domes are in contact. For each interdome spacing, the extinction spectrum was measured using a broadband reflection instrumentation, and finite-difference-time-domain (FDTD) simulation was used to model the local electric field distribution associated with the resonances. Based on these studies, we predict that nanodome array devices with gap between 14 nm to 20 nm provide optimal label-free capture affinity biosensing performances, where the dipole resonance mode exhibits the highest overall surface sensitivity, as well as the lowest limit of detection.