Hastelloy X is a Ni-Cr-Fe-Mo alloy with significant carbide content that can be difficult to etch due to its corrosion resistance. Etching reveals the austenitic matrix, grain boundaries, and carbide distribution. Three etchants are recommended:
Glyceregia (Chemical Etching) - Primary choice for general microstructure:
- Composition: 15ml HCl + 5ml HNO₃ + 10ml glycerol. Add acids to glycerol slowly with stirring.
- Application: Immerse or swab for 10-30 seconds. Prepare fresh — decomposes within hours. The glycerol moderates the reaction rate for controlled etching.
- Reveals: Grain boundaries, twin boundaries, and carbide distribution in the austenitic matrix.
- Rinse: Immediately with water, then ethanol. Dry with compressed air or warm air to avoid staining.
Adler's Etchant (Chemical Etching) - Very effective for Hastelloy alloys:
- Composition: 45g FeCl₃ + 9g copper ammonium chloride (CuCl₂·2NH₄Cl) + 150ml HCl + 75ml H₂O
- Application: Immerse for 5-15 seconds. More aggressive than Glyceregia — use when Glyceregia provides insufficient contrast.
- Reveals: Grain boundaries, carbides, and TCP phases with strong contrast.
- Rinse: Immediately with water, then ethanol. Dry with compressed air.
Electrolytic 10% Oxalic Acid (Electrolytic Etching) - For controlled, selective etching:
- Composition: 10g oxalic acid dihydrate in 100ml H₂O
- Application: Electrolytic — sample as anode, stainless steel cathode. Apply 6V DC for 5-30 seconds. Voltage control allows precise etching depth.
- Reveals: Grain boundaries, M₆C and M₂₃C₆ carbides, and secondary phases.
- Rinse: Immediately with water, then ethanol. Dry with compressed air.
Etching Strategy:
- Start with Glyceregia for general microstructure and carbide distribution
- If Glyceregia gives insufficient contrast (common with Hastelloy), use Adler's Etchant
- Use electrolytic 10% oxalic for controlled, selective etching (carbide identification, sensitization)
- Always clean and degrease before etching — residual polishing compound will interfere
- Use short initial etch times, check under the microscope, and repeat if needed
Safety: Glyceregia produces toxic fumes — use in fume hood. Adler's contains concentrated HCl — fume hood required. Electrolytic etching requires proper electrical setup. Wear gloves, safety glasses, and lab coat for all etchants.