The epitaxial lift-off (ELO) process based on selectively etching a thin sacrificial AlAs layer from GaAs substrate was performed using high-concentrated aqueous hydrofluoric (HF) etchant. However, because of using the wet etching method, the traditional ELO process has many drawbacks and limitations. Supercritical fluids (SCFs) naturally have the characteristics of low viscosity, high diffusivity, and zero surface tension. Therefore, the development of a gas-phase-like dry etching method based on mixing HF into CO2 and operating the mixture of HF/CO2 in SCFs condition as etchant is hereby proposed to overcome those bottlenecks existing in traditional wet ELO processes. However, there are no available experimental results for etching AlAs layers by HF in SCFs yet. Therefore, a HF-compatible corrosion-resistant high-pressure system was designed and built up to perform the idea. The capabilities of etching sample in supercritical CO2 (scCO2) had been systemically investigated under various pressures (2000–3000 psi) and temperatures (40–60[Formula: see text]C). Besides, the etching performances separately conducted by using aqueous-HF and anhydrous HF/Pyridine as the source etchant and mixing with scCO2 at a fixed temperature, pressure and etching time were also examined and compared under different equivalent HF concentrations. An evaluation of using acetone as the co-solvent mixed with HF/scCO2 mixture for enhancing the etch rate in different volume ratio of HF/co-solvent was further investigated and discussed. With this system, we demonstrate releasing a size of [Formula: see text] (width × length) and 3 [Formula: see text]m-thick free-standing GaAs sheet from a 150 nm AlAs sacrificial layer by the etching sample in HF/scCO2 mixture. The released GaAs sheet was also successfully transferred to a flexible PET substrate by using a PDMS stamp and an adhesive layer of NOA61.
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