Abstract

In the last decades, Raman spectroscopy has become an important tool to identify and investigate minerals, gases, glasses, and organic material at room temperature. In combination with high-temperature and high-pressure devices, however, the in situ investigation of mineral transformation reactions and their kinetics is nowadays also possible. Here, we present a novel approach to in situ studies for the sintering process of silicate ceramics by hyperspectral Raman imaging. This imaging technique allows studying high-temperature solid-solid and/or solid-melt reactions spatially and temporally resolved, and opens up new avenues to study and visualize high-temperature sintering processes in multi-component systems. After describing in detail the methodology, the results of three application examples are presented and discussed. These experiments demonstrate the power of hyperspectral Raman imaging for in situ studies of the mechanism(s) of solid-solid or solid-melt reactions at high-temperature with a micrometer-scale resolution as well as to gain kinetic information from the temperature- and time-dependent growth and breakdown of minerals during isothermal or isochronal sintering.

Highlights

  • In the last decades, Raman spectroscopy has become one of the most important analytical tools for a wide range of research areas in all sub-disciplines of physics, chemistry, biology, geosciences, and medicine

  • In a recently published study, we reported the first results of sintering experiments using confocal hyperspectral Raman imaging (CHRI) to in situ study high-temperature, solid-state reactions in kaolin-based green bodies [24]

  • We describe our novel approach to in situ study the sintering process of silicate ceramics by hyperspectral Raman imaging in little more detail

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Summary

Introduction

Raman spectroscopy has become one of the most important analytical tools for a wide range of research areas in all sub-disciplines of physics, chemistry, biology, geosciences, and medicine. Raman imaging enables a rapid, routinely practicable, non-destructive food quality and safety evaluation [3] and has turned into a novel clinical diagnostic tool in biomedical applications [4] It facilitates the investigation of heterogeneous systems and thereby reveals a wealth of chemical and physical information about the chemical composition, short-range atomic structure, structural strain, crystallite orientation [5]. We combined the advantages of in situ high-temperature Raman spectroscopy with the possibility of 2-dimensional Raman imaging with a micrometer-scale resolution as a powerful tool for the in situ investigation of solid state sintering processes. The power of in situ Raman imaging for studying high-temperature sintering reactions is briefly demonstrated by three application examples

Analytical Details
Experimental Series
Sample Preparation
Heating Stage and Temperature Calibration
Map Programming
Hyperspectral
Data Reduction
Factors Affecting Phase Quantification
A ofof three hyperspectral between838
10. Normalized intensities themain mainRaman
Mineral Reactions During Firing and Cooling
Isothermal Mineral Reactions and Grain Growth
SiO4the program
In Situ Observations of the Migration of Solid-Solid Reaction Fronts
SiO4 thick α’L-Ca2SiO
Future
Findings
Conclusions
Full Text
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