A method is reported for the synthesis of single-atom-thick gold (goldene) by exfoliating it from a nanolaminated MAX phase, Ti₃AuC₂, through wet-chemical etching of the Ti₃C₂ carbide layers. The process involves using Murakami's reagent with surfactants such as CTAB or cysteine to remove the Ti₃C₂ layers, resulting in free-standing goldene sheets. The goldene layers exhibit a 9% lattice contraction compared to bulk gold and show increased Au 4f binding energy by 0.88 eV. While ab initio molecular dynamics simulations indicate that goldene is inherently stable, experimental observations show some curling and agglomeration, which can be mitigated by surfactants. X-ray photoelectron spectroscopy confirms the Au 4f binding energy shift. The study highlights the potential of goldene for applications in plasmonics, catalysis, and electronics due to its unique properties. The synthesis method is scalable and hydrofluoric acid-free, and the goldene sheets are stable and planar. The research also explores the possibility of preparing goldene from other non-van der Waals Au-intercalated MAX phases, including developing etching schemes. The study provides insights into the electronic properties of goldene, showing that it has a different electronic structure compared to bulk gold. The results demonstrate the feasibility of producing free-standing, single-atom-thick gold sheets, which could have significant implications for future applications in nanotechnology and materials science.A method is reported for the synthesis of single-atom-thick gold (goldene) by exfoliating it from a nanolaminated MAX phase, Ti₃AuC₂, through wet-chemical etching of the Ti₃C₂ carbide layers. The process involves using Murakami's reagent with surfactants such as CTAB or cysteine to remove the Ti₃C₂ layers, resulting in free-standing goldene sheets. The goldene layers exhibit a 9% lattice contraction compared to bulk gold and show increased Au 4f binding energy by 0.88 eV. While ab initio molecular dynamics simulations indicate that goldene is inherently stable, experimental observations show some curling and agglomeration, which can be mitigated by surfactants. X-ray photoelectron spectroscopy confirms the Au 4f binding energy shift. The study highlights the potential of goldene for applications in plasmonics, catalysis, and electronics due to its unique properties. The synthesis method is scalable and hydrofluoric acid-free, and the goldene sheets are stable and planar. The research also explores the possibility of preparing goldene from other non-van der Waals Au-intercalated MAX phases, including developing etching schemes. The study provides insights into the electronic properties of goldene, showing that it has a different electronic structure compared to bulk gold. The results demonstrate the feasibility of producing free-standing, single-atom-thick gold sheets, which could have significant implications for future applications in nanotechnology and materials science.