Advanced Characterization of Slags and Refractory Bricks Using Electron Backscatter Diffraction
Numerous studies have been conducted to determine changes that occur in slag that cause a rapid change in viscosity, but these studies have been limited by the inability to characterize/identify the phases present in the slag. Rapid freezing of slag in entrained gasifiers and slagging combustion systems can cause a shutdown of the system. The reactions occurring in slag that result in rapid freezing of slags are not well understood. It is believed that electron backscatter diffraction (EBSD) can be used to analyze slags and aid in their characterization although its use has not been found in literature. The EBSD technique allows particle-by-particle mineralogy based on diffraction patterns generated by the electron beam when the sample is tilted to a high angle. The diffraction pattern (Kikuchi bands) can only come from crystalline phases, which makes this technique ideally suited to study crystal formation in slags where oftentimes the crystals are very small and a reasonable chemical analysis cannot be made by conventional energy-dispersive spectrometry (EDS) methods in the scanning electron microscope. The ability to have mineralogical data based on the crystalline structure of a phase rather than a chemical analysis by EDS allows much better interpretation of the temperature regimes in which specific phases tend to form. Knowing the type and relative amounts of a phase crystallizing in a slag is critical in predicting the viscosity of a slag at a given temperature. Six slag samples were selected based on the parent coal. Unfortunately, none of the slags appeared to have any crystalline material associated with them. The funding for this project was not adequate for generating more slags from the various coal types. For this reason, sample archives were searched for those containing slags that were not rapidly quenched. A slag from a bituminous coal was found to contain several dendritic crystals (10 {mu}m to 50 {mu}m in size) that formed near the edges of the slag. Analysis of these crystals identified the crystalline phase epidote - Ca{sub 2}Al{sub 2}O(Al, Fe{sup 3+})OH(Si{sub 2}O{sub 7})(SiO{sub 4}). The identification could not have been performed from EDS alone because of Ca deficiency. However, looking at the crystal structure combined with EDS shows that the phase present is a Ca-deficient epidote. From this information, a temperature range of formation was determined. This gives a good example of the additional clarity that can be derived from utilizing EBSD. Evaluation of corrosion products by EBSD at the refractory brick and slag interface did reveal penetration and corrosion of slag into the brick through examination of crystalline phases alone. The degree of corrosion was dependent on the type of refractory and chemical makeup of the slag. This technique has not been used before to analyze slags and slag/refractory interactions. More work needs to be performed to better utilize EBSD for this type of analysis. This project demonstrates that the method is a valid technique that can be used to characterize slags and their interactions with refractory materials.
- Research Organization:
- Univ. of North Dakota, Grand Forks, ND (United States)
- Sponsoring Organization:
- USDOE
- DOE Contract Number:
- FC26-98FT40320
- OSTI ID:
- 984654
- Country of Publication:
- United States
- Language:
- English
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