Effect of acid etching on tridimensional microstructure of etchable CAD/CAM materials

Evaluate if etching protocols affect superficial/internal microstructural integrity of CAD/CAM ceramic materials.

Sixty blocks (3×3×3mm) of IPS/Empress-LEU, IPS/e.max-LDC (Ivoclar-Vivadent) and Enamic-PIC (VITA) were used. Lateral surfaces from each block were isolated with Teflon strip and petroleum jelly to keep them untouched. Specimens were distributed into 6 groups (n=10): 1. no treatment (C); 2. hydrofluoric acid (HF) 5%, 20s (HF5%20s); 3. HF5%60s; 4. HF10%20s; 5. HF10%60s; 6. Monobond Etch&Prime (MBEP). Surface roughness (Sa) and 3D profile were obtained using a confocal-laser-optical-microscope (LEXT OLS 4000, Olympus), while element ratios (Si/K for LEU and LDC; Si/C for PIC) were recorded using energy dispersive spectroscopy (EDS). Superior (treated) and lateral (non-treated) surfaces were analyzed using scanning electron microscopy (SEM) (JSM 5600 LV, JEOL). Etching depth was measured on lateral surfaces. Data were submitted to ANOVA-One-Way and Tukey test (α=0.05).

For LEU, only HF10% treatments produced statistically different roughness values and Si/K ratios compared to C group. Regarding LDC and PIC, groups HF5%60s and HF10% showed higher roughness values than C group. In the case of PIC, all treatments (except MBEP) produced lower Si/C ratios than C group. All treatments (except MBEP) produced higher etching depth values than C group for all materials, being HF10%60s the highest (LEU:403.2±11.4μm; LDC:617.4±75.7; PIC:291.6±6.5μm). HF10% produced more aggressive etching morphology patterns on superior and lateral surfaces (SEM). Treatments MBEP and HF5%20s, produced the least aggressive structural alterations. Acid etching produces superficial and internal alterations on ceramics' structural configuration.

Aggressive etching protocols of glass-ceramics may cause internal material loss, consequently, milder etching is recommended to treat those materials before adhesion procedures.