We introduce optically clear and resilient free-form micro-optical components of pure (non-photosensitized) organic-inorganic SZ2080 material made by femtosecond 3D laser lithography (3DLL). This is advantageous for rapid printing of 3D micro-/nano-optics, including their integration directly onto optical fibers. A systematic study of the fabrication peculiarities and quality of resultant structures is performed. Comparison of microlens resiliency to continuous wave (CW) and femtosecond pulsed exposure is determined. Experimental results prove that pure SZ2080 is ∼20 fold more resistant to high irradiance as compared with standard lithographic material (SU8) and can sustain up to 1.91 GW/cm2 intensity. 3DLL is a promising manufacturing approach for high-intensity micro-optics for emerging fields in astro-photonics and atto-second pulse generation. Additionally, pyrolysis is employed to homogeneously shrink structures up to 40% by removing organic SZ2080 constituents. This opens a promising route towards downscaling photonic lattices and the creation of mechanically robust glass-ceramic microstructures.
Fabrication of a true-3D inorganic ceramic with resolution down to the nanoscale (∼100 nm) using a sol–gel resist precursor is demonstrated. This method has an unrestricted free-form capability, control of the fill-factor, and high fabrication throughput. A systematic study of the proposed approach based on ultrafast laser 3D lithography of organic–inorganic hybrid sol–gel resin followed by a heat treatment enabled the formation of inorganic amorphous and crystalline composites guided by the composition of the initial resin. The achieved resolution of 100 nm was obtained for 3D patterns of complex free-form architectures. Fabrication throughput of 50 × 103 voxels per second is achieved; voxel – a single volume element recorded by a single pulse exposure. A post-exposure thermal treatment was used to form a ceramic phase, the composition and structure of which were dependent on the temperature and duration of the heat treatment as revealed by Raman micro-spectroscopy. The X-ray diffraction (XRD) showed a gradual emergence of the crystalline phases at higher temperatures with a signature of cristobalite SiO2, a high-temperature polymorph. Also, a tetragonal ZrO2 phase known for its high fracture strength was observed. This 3D nano-sintering technique is scalable from nanoscale to millimeter dimensions and opens a conceptually novel route for optical 3D nano-printing of various crystalline inorganic materials defined by an initial composition for diverse applications for microdevices designed to function in harsh physical and chemical environments and at high temperatures.
A pilot study on laser 3D printing of inorganic free-form micro-optics is experimentally validated. Ultrafast laser direct-write (LDW) nanolithography is employed for structuring hybrid organic-inorganic material SZ2080TM followed by high-temperature calcination post-processing. The combination allows the production of 3D architectures and the heat-treatment results in converting the material to inorganic substances. The produced miniature optical elements are characterized and their optical performance is demonstrated. Finally, the concept is validated for manufacturing compound optical components such as stacked lenses. This is an opening for new directions and applications of laser-made micro-optics under harsh conditions such as high intensity radiation, temperature, acidic environment, pressure variations, which include open space, astrophotonics, and remote sensing.
Selective laser etching (SLE) is a technique that allows the fabrication of arbitrarily shaped glass micro-objects. In this work, we show how the capabilities of this technology can be improved in terms of selectivity and etch rate by applying an etchant solution based on a Potassium Hydroxide, water, and isopropanol mixture. By varying the concentrations of these constituents, the wetting properties, as well as the chemical reaction of fused silica etching, can be changed, allowing us to achieve etching rates in modified fused silica up to 820 μm/h and selectivity up to ∼3000. This is used to produce a high aspect ratio (up to 1:1000), straight and spiral microfluidic channels which are embedded inside a volume of glass. Complex 3D glass micro-structures are also demonstrated.
Hydraulic calcium silicate-based (HCS) sealers have recently gained tremendous popularity due to their unique properties. However, their removal during endodontic retreatment is challenging. The solvent, which could chemically deteriorate the material, would be highly desirable for endodontic retreatment procedures. This preliminary study assessed the interplay and dissolving capability of 10% and 20% citric acid, compared to 17% EDTA, on commonly used HCS sealers (AH Plus Bioceramic Sealer, Bio-C Sealer, BioRoot RCS, TotalFill BC Sealer), and evaluated the potential impact of these solutions on root dentin structure. The interaction between tested sealers and irrigating solutions was photographed, and solubility-related mass changes were determined. The surface morphology of treated filling materials and dentin was evaluated using a scanning electron microscope (SEM). One-way analysis of variance (ANOVA) along with Tukey’s test were used to detect the statistically significant differences among groups at the confidence level of 0.95. Intense gas release was observed during the interaction of HCS materials and citric acid, with no evidently visible “bubbling” after the immersion in EDTA. The mass loss of HCS sealers equally confirmed the significantly higher dissolving characteristics of 10% and 20% citric acid solutions compared to EDTA. The surface structural changes, associated with pore and crack formation, were mainly seen for HCS sealers exposed to citric acid. Meanwhile, no severe erosion was detected for dentin after root canal preparation with 10% and 20% citric acid solutions. These findings demonstrate that citric acid has the potential to dissolve HCS sealers with minimal or no negative impact on root dentin, suggesting citric acid as a solvent for HCS sealers in endodontic retreatment procedures.