Kang, Seokwon (2012-05). Thermal Bimorph Micro-Cantilever Based Nano-Calorimeter for Sensing of Energetic Materials. Doctoral Dissertation.
The objective of this study is to develop a robust portable nano-calorimeter sensor for detection of energetic materials, primarily explosives, combustible materials and propellants. A micro-cantilever sensor array is actuated thermally using bi-morph structure consisting of gold (Au: 400 nm) and silicon nitride (Si3N4: 600 nm) thin film layers of sub-micron thickness. An array of micro-heaters is integrated with the microcantilevers at their base. On electrically activating the micro-heaters at different actuation currents the microcantilevers undergo thermo-mechanical deformation, due to differential coefficient of thermal expansion. This deformation is tracked by monitoring the reflected ray from a laser illuminating the individual microcantilevers (i.e., using the optical lever principle). In the presence of explosive vapors, the change in bending response of microcantilever is affected by the induced thermal stresses arising from temperature changes due to adsorption and combustion reactions (catalyzed by the gold surface). A parametric study was performed for investigating the optimum values by varying the thickness and length in parallel with the heater power since the sensor sensitivity is enhanced by the optimum geometry as well as operating conditions for the sensor (e.g., temperature distribution within the microcantilever, power supply, concentration of the analyte, etc.). Also, for the geometry present in this study the nano-coatings of high thermal conductivity materials (e.g., Carbon Nanotubes: CNTs) over the microcantilever surface enables maximizing the thermally induced stress, which results in the enhancement of sensor sensitivity. For this purpose, CNTs are synthesized by post-growth method over the metal (e.g., Palladium Chloride: PdCl2) catalyst arrays pre-deposited by Dip-Pen Nanolithography (DPN) technique. The threshold current for differential actuation of the microcantilevers is correlated with the catalytic activity of a particular explosive (combustible vapor) over the metal (Au) catalysts and the corresponding vapor pressure. Numerical modeling is also explored to study the variation of temperature, species concentration and deflection of individual microcantilevers as a function of actuation current. Joule-heating in the resistive heating elements was coupled with the gaseous combustion at the heated surface to obtain the temperature profile and therefore the deflection of a microcantilever by calculating the thermally induced stress and strain relationship. The sensitivity of the threshold current of the sensor that is used for the specific detection and identification of individual explosives samples - is predicted to depend on the chemical kinetics and the vapor pressure. The simulation results showed similar trends with the experimental results for monitoring the bending response of the microcantilever sensors to explosive vapors (e.g., Acetone and 2-Propanol) as a function of the actuation current.