Commercially Pure Titanium Grade 4 is the strongest CP grade with the highest oxygen content. The microstructure is single-phase alpha with equiaxed grains — there is no beta phase. The higher strength compared to Grades 1-3 allows slightly more aggressive etching.
Kroll's Reagent (Chemical Etching) - Standard etchant:
- 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 5-10 seconds. Grade 4 tolerates standard Kroll's better than lower CP grades due to higher strength.
- Reveals: Equiaxed alpha grain boundaries and annealing twins. Grain size assessment per ASTM E112.
- Rinse: Immediately with water, then ethanol. Dry with compressed air.
Modified Kroll's Reagent (Chemical Etching) - For more controlled etching:
- Composition: 1ml HF + 3ml HNO₃ + 100ml H₂O
- Application: Swab for 10-30 seconds. Use when more controlled grain boundary etching is needed or for grain size comparison studies.
- Reveals: Alpha grain boundaries with finer contrast control than standard Kroll's.
Etching Strategy:
- No beta phase present — all grains are alpha; contrast comes from grain boundary etching and crystallographic orientation
- Grade 4 tolerates standard Kroll's better than Grades 1-3 due to higher oxygen-strengthened matrix
- Polarized light on unetched or lightly etched surfaces reveals alpha grain orientation colors
- For grain size measurement, ensure consistent etch across the entire sample surface
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.