Abstract

To optimize the operation and functioning of high temperature systems such as slagging gasifiers, coal boilers and glass/steel melters, it is important to monitor corrosion and erosion of refractory used in such systems. Corrosion test strategies are generally based on continuous gravimetric and chemical reactivity monitoring at operational temperatures (750°-1500°C). Both thermocouples and failure sensors and arrays would be useful to monitor the health of any refractory or coatings in these systems. Many of such type of sensors are installed into the systems through open access ports within the refractory; however, there are some disadvantages of this approach where corrosive/erosive gas and molten materials can penetrate and compromise the system. The current work presents the development and performance demonstration of smart refractory with embedded high temperature sensors such as thermocouples, thermistors, and various spallation/crack monitoring sensors, which may be used within a variety of refractory brick in different high temperature processes and applications.The main feature of this technology is that electroceramic based sensors are embedded into smart refractory without significantly impact to the intrinsic properties of the refractory. This technology circumvents the need to insert an isolated monolithic, stand-alone sensor into the refractory via an access port. This technological approach guarantees the integrity and the chemical stability of the materials used in the sensor fabrication within the harsh environment and does not introduce molten material (such as slag) penetration pathways within the refractory. One interesting and important aspect of this innovation is that these embedded sensors can be used to in situ monitoring processes such as chemical reactions and at the same time give information and a deeper understanding of the corrosion and erosion process of the refractory within the system.As stated above, the objective of our work is to develop high-temperature sensors composed of electroceramic materials that are chemically stable at high temperatures (750°-1500°C) and high pressures (up to 1000 psi) that can be used in monitoring corrosion and erosion process in refractory used in high energy systems. The high-temperature sensors investigated in this work were composed of various oxide composites directly embedded into the refractory oxides. The composites used for this work were synthesized by a mixed-oxide route. Metal oxides were inserted within a matrix material composed of refractory oxides (Al2O3, ZrO2, etc.). The physical and electrical properties were specifically manipulated by altering the level of percolation of the conductive species (metal oxides) within the refractory constituent (refractory oxide).Prior to the development of the high-temperature sensors, the oxides composites developed in this study were sintered up to 1600°C under oxidizing atmosphere in order to investigate densification, microstructural evolution, phase development, and their thermoelectrical performance as a function of the composition. The 4-point DC conductivity measurements were performed between 100°-1500°C. The sensors were fabricated from the composite materials by 3D-printing or screen-printing methods into the refractory brick during the consolidation process.An example of one of these embedded sensors consisted of an electroceramic-based thermocouple fabricated with two separate oxide composite compositions which were patterned to produce a couple within the interior of a refractory matrix. The thermocouple successfully displayed thermoelectric voltage trend (as a function of temperature), and the voltage was 220.0 mV around 1400 °C.Corrosion tests on the refractory embedded sensors were performed. To evaluate corrosion in the refractory brick an in-house glass composition was prepared and pressed into pellets and delivered into a pre-cut cavity in the brick. Corrosion experiments results showed the glass penetrated the brick over a 90 h period, and the penetration of the glass through the brick could be monitored by both a amperometric and voltametric based sensor. With this experiment, it was demonstrated that the embedded sensor could dynamically monitor the corrosion process. Acknowledgements: This work was supported by the United States Department of Energy (DOE) through the research project grant (DE-FE0031825). The authors would also like to acknowledge the technical support of Dr. Qiang Wang, Dr. Marcela Redigolo and Mr. Harley Hart of WVU Shared Research Facilities (SRF) for assistance in characterization and technical input.

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