In the past decades, increased human population and activities have introduced a large amount of pollutants into the environment. Various types of conventional analytical instruments were used for monitoring the emitted chemicals with low detection limit, high accuracy, and discrimination power. However, many of these methods are laboratory-based owing to sample collection, transportation, extraction, and purification steps. To make real-time on-site monitoring possible, miniaturized sensors with various integrated elements were developed. One of the most well-known strategies is to utilize nanostructured materials with enhanced sensing properties for those devices. For a majority of the current state of art devices, the synthesis of nanostructured materials and device integration are done separately, that is, "synthesis first and then integration" approach which involves two separate process steps. However, this approach comes with some disadvantages such as misalignment, contamination, as well as disconnection between nanomaterials and electrodes. To overcome the aforementioned technical challenge, several synthesis methods were developed and validated for in-situ integration of nanostructured metal and metal oxide materials for environmental sensors in this work. The electroplating technique combined with photolithography was used to make the predefined metal electrodes. Then, with subsequent post-treatments, nanostructured metals and metal oxides could be produced in-situ and directly integrated in the electrodes without any extra transfer process steps. In the process of developing a phosphate sensor, nanofibrous Co electrodes were fabricated by pulsed electroplating of Co-Cu alloy and dealloying the Cu component. A linear potentiometric response to phosphate in the 10-5 to 10-2 M concentration range was obtained which validated the sensor's function. A mechanism based on mixed potential response was proposed to elucidate the Co electrode behavior in aqueous solutions with varying pH conditions and optimum pH ranges for working devices were proposed. In addition to the alloying and dealloying method, the template assisted electroplating method was also investigated. A nanoporous Co-Cu electrode fabricated by electroplating through a sacrificial glass fiber template was obtained. A linear amperometric response to phosphate with suppressed oxygen interference was achieved in a 10-5 to 10-2 M concentration range of phosphate. An analysis of the cyclic voltammetry characterization results provided a direction for further exploring an optimized electrode polarization potential range for suppressing oxygen interference while maintaining a good sensitivity to phosphate. Based on this result, we improved the fabrication process with another template: in-situ hydrothermally grown ZnO nanoflakes on the electrode surface, as a template for uniform nanostructured Co electroplating. The cyclic voltammetry characterization of the fabricated electrode showed an amperometric response in the range of 10-6 to 10-2 M of phosphate where the limit of detection (LOD) was enhanced compared with the previous work. For the flammable gas sensor development, the in-situ oxidation of Cu was utilized to form nanowires for sensing electrode fabrication. Multiple CuO nanowires were synthesized in-situ on the electroplated interdigitated Cu electrodes on a hotplate at 500 °C in air. The nanowires were successfully integrated as a sensing element into the device, forming bridges between two electrodes. The sensor's behavior was characterized by a current-voltage measurement. Simple processing parameters could be utilized for controlling the electrode morphologies and determining the characteristics of contacts - Schottky or Ohmic - at the electrode interface. A hypothesis was proposed to explain the transition phenomenon between Schottky and Ohmic contact modes, providing an important baseline for future device design and fabrication. Finally, the fabricated sensor was tested for a flammable gas detection using saturated ethanol vapor at room temperature, which implicates a low power consumption gas sensor without elevating the sensor temperature unlike traditional gas sensors.
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Cho, Hyoung Jin
Doctor of Philosophy (Ph.D.)
College of Engineering and Computer Science
Materials Science Engineering
Materials Science and Engineering
Length of Campus-only Access
Doctoral Dissertation (Open Access)
Wang, Xiaochen, "Electrode Integration of Nanostructured Metal and Metal Oxide Materials Based on in-situ Growth Methods for Environmental Sensors" (2017). Electronic Theses and Dissertations, 2004-2019. 5937.