Titanium Matrix Composite (TMC) requires a specialized etching approach. Kroll's Reagent etches only the titanium matrix — SiC fiber reinforcement is chemically inert to HF-based etchants. Examine the unetched polished surface first to assess fiber distribution, interface integrity, and reaction zone thickness before etching.
Kroll's Reagent (Chemical Etching) - For titanium matrix only:
- Composition: 2-3ml HF + 5ml HNO₃ + 100ml H₂O
- Preparation: Add acids to water slowly with stirring in a plastic container (HF attacks glass). Prepare fresh for best results.
- Application: Swab for 5-15 seconds. Etchant attacks titanium matrix only — SiC fibers and reaction zone remain unaffected.
- Reveals: Alpha and beta phases in the titanium matrix between fibers. Grain structure near and away from fiber/matrix interfaces. Reaction zone (typically TiC + Ti₅Si₃) visible as a distinct ring around each fiber.
- Rinse: Immediately with water, then ethanol. Dry with compressed air.
Unetched Examination - Essential first step for TMC:
- Method: Bright-field and DIC microscopy on as-polished surface.
- Reveals: Fiber distribution and spacing, fiber damage from processing, consolidation voids, and fiber/matrix interface reaction zone thickness. Many critical TMC quality assessments require unetched examination.
Etching Strategy:
- Always examine unetched first — fiber distribution and interface reaction zone are best assessed before etching
- Kroll's etches only the Ti matrix; differential etching at the fiber/matrix interface creates topographic relief
- Avoid aggressive or prolonged etching which can undercut the matrix around fibers, causing fiber pullout
- SEM/EDS useful for characterizing the fiber/matrix reaction zone composition
Safety: HF is extremely hazardous — always use in a fume hood with HF-rated gloves, face shield, and lab coat. Have calcium gluconate gel available. Store all HF solutions in plastic containers.