Laser additive manufacturing of Si/ZrO2 tunable crystalline phase 3D nanostructures

Abstract

The current study is directed to the rapidly developing field of inorganic material 3D object production at nano-/micro scale. The fabrication method includes laser lithography of hybrid organic-inorganic materials with subsequent heat treatment leading to a variety of crystalline phases in 3D structures. In this work, it was examined a series of organometallic polymer precursors with different silicon (Si) and zirconium (Zr) molar ratios, ranging from 9:1 to 5:5, prepared via sol-gel method. All mixtures were examined for perspective to be used in 3D laser manufacturing by fabricating nano-and mi-cro-feature sized structures. Their spatial downscaling and surface morphology were evaluated depending on chemical composition and crystallographic phase. The appearance of a crystalline phase was proven using single-crystal X-ray dif-fraction analysis, which revealed a lower crystallization temperature for microstructures compared to bulk materials. Fabricated 3D objects retained a complex geometry without any distortion after heat treatment up to 1400 °C. Under the proper conditions, a wide variety of crystalline phases as well as zircon (ZrSiO4-a highly stable material) can be ob-served. In addition, the highest new record of achieved resolution below 60 nm has been reached. The proposed prepar-ation protocol can be used to manufacture micro/nano-devices with high precision and resistance to high temperature and aggressive environment.