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Thermochemical interactions between calcium–magnesium–aluminosilicate (CMAS) glass and an environmental barrier coating of ytterbium disilicate (Yb2Si2O7) and ytterbium monosilicate (Yb2SiO5) were investigated. Top coats were deposited by plasma spray-physical vapor deposition onto silicon carbide substrates. CMAS powder was prepared as a glass and cast into a tape to yield a CMAS loading of ~29 mg/cm2. Samples were heat treated with CMAS at 1300 °C for 1–10 h or at 1400 °C for 1 h in air. Polished specimen cross-sections were characterized using scanning electron microscopy, X-ray diffraction, X-ray energy-dispersive spectroscopy, and transmission electron microscopy to evaluate resulting microstructures, phases, and compositions at CMAS/Yb2Si2O7 interfaces. Coatings exposed at 1300 °C—10 h and 1400 °C—1 h were fully infiltrated and compromised by CMAS. Dissolution of ytterbium silicate into molten CMAS followed by precipitation of cyclosilicate, silicocarnotite, and Yb2Si2O7 at 1300 °C and Yb2Si2O7 at 1400 °C enabled CMAS to effectively infiltrate top coats, rendering the predominantly Yb2Si2O7 coating ineffective at arresting molten CMAS degradation.