The effect of various HF‐based etching processes on the laser damage resistance of scratched fused silica surfaces has been investigated. Conventionally polished and subsequently scratched fused silica plates were treated by submerging in various HF‐based etchants (HF or NH4F:HF at various ratios and concentrations) under different process conditions (e.g., agitation frequencies, etch times, rinse conditions, and environmental cleanliness). Subsequently, the laser damage resistance (at 351 or 355 nm) of the treated surface was measured. The laser damage resistance was found to be strongly process dependent and scaled inversely with scratch width. The etching process was optimized to remove or prevent the presence of identified precursors (chemical impurities, fracture surfaces, and silica‐based redeposit) known to lead to laser damage initiation. The redeposit precursor was reduced (and hence the damage threshold was increased) by: (1) increasing the SiF62− solubility through reduction in the NH4F concentration and impurity cation impurities, and (2) improving the mass transport of reaction product (SiF62−) (using high‐frequency ultrasonic agitation and excessive spray rinsing) away from the etched surface. A 2D finite element crack‐etching and rinsing mass transport model (incorporating diffusion and advection) was used to predict reaction product concentration. The predictions are consistent with the experimentally observed process trends. The laser damage thresholds also increased with etched amount (up to ∼30 μm), which has been attributed to: (1) etching through lateral cracks where there is poor acid penetration, and (2) increasing the crack opening resulting in increased mass transport rates. With the optimized etch process, laser damage resistance increased dramatically; the average threshold fluence for damage initiation for 30 μm wide scratches increased from 7 to 41 J/cm2, and the statistical probability of damage initiation at 12 J/cm2 of an ensemble of scratches decreased from ∼100 mm−1 of scratch length to ∼0.001 mm−1.

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a b s t r a c tThe effects of HF/NH 4 F, wet chemical etching on the morphology of individual surface fractures (indentations, scratches) and of an ensemble of surface fractures (ground surfaces) on fused silica glass has been characterized. For the individual surface fractures, a series of static or dynamic (sliding) Vickers and Brinnell indenters were used to create radial, lateral, Hertzian cone and trailing indentation fractures on a set of polished fused silica substrates which were subsequently etched. After short etch times, the visibility of both surface and subsurface cracks is significantly enhanced when observed by optical microscopy. This is attributed to the increased width of the cracks following etching, allowing for greater optical scatter at the fracture interface. The removal of material during etching was found to be isotropic except in areas where the etchant has difficulty penetrating or in areas that exhibit significant plastic deformation/ densification. Isolated fractures continue to etch, but will never be completely removed since the bottom and top of the crack both etch at the same rate. The etching behavior of ensembles of closely spaced cracks, such as those produced during grinding, has also been characterized. This was done using a second set of fused silica samples that were ground using either fixed or loose abrasives. The resulting samples were etched and both the etch rate and the morphology of the surfaces were monitored as a function of time. Etching results in the formation of a series of open cracks or cusps, each corresponding to the individual fractures originally on the surface of the substrate. During extended etching, the individual cusps coalesce with one another, providing a means of reducing the depth of subsurface damage and the peak-to-valley roughness. In addition, the material removal rate of the ground surfaces was found to scale with the surface area of the cracks as a function of etch time. The initial removal rate for the ground surface was typically 3.5Â the bulk etch rate. The evolving morphology of ground surfaces during etching was simulated using an isotropic finite difference model. This model illustrates the importance that the initial distributions of fracture sizes and spatial locations have on the evolution of roughness and the rate at which material is removed during the etching process. The etching of ground surfaces can be used during optical fabrication to convert subsurface damage into surface roughness thereby reducing the time required to produce polished surfaces that are free of subsurface damage.

The distribution and characteristics of surface cracks (i.e., sub-surface damage or scratching) on fused silica formed during grinding/polishing resulting from the addition of rogue particles in the base slurry has been investigated. Fused silica samples (10 cm diameter x 1 cm thick) were: 1) ground by loose abrasive grinding (alumina particles 9-30 µm) on a glass lap with the addition of larger alumina particles at various concentrations with mean sizes ranging from 15-30 µm, or 2) polished (using 0.5 µm cerium oxide slurry) on various laps (polyurethanes pads or pitch) with the addition of larger rogue particles (diamond (4-45 µm), pitch, dust, or dried Ceria slurry agglomerates) at various concentrations. For the resulting ground samples, the crack distributions of the as-prepared surfaces were determined using a polished taper technique. The crack depth was observed to: 1) increase at small concentrations (>10 -4 fraction) of rogue particles; and 2) increase with rogue particle concentration to crack depths consistent with that observed when grinding with particles the size of the rogue particles alone. For the polished samples, which were subsequently etched in HF:NH 4 F to expose the surface damage, the resulting scratch properties (type, number density, width, and length) were characterized. The number density of scratches increased exponentially with the size of the rogue diamond at a fixed rogue diamond concentration suggesting that larger particles are more likely to lead to scratching. The length of the scratch was found to increase with rogue particle size, increase with lap viscosity, and decrease with applied load. At high diamond concentrations, the type of scratch transitioned from brittle to ductile and the length of the scratches dramatically increased and extended to the edge of the optic. The observed trends can explained semi-quantitatively in terms of the time needed for a rogue particle to penetrate into a viscoelastic lap. The results of this study provide useful insights and 'rules-of-thumb' relating scratch characteristics observed on surfaces during optical glass fabrication to the characteristics rogue particles causing them and their possible source.