This study focuses on experiments of Au and Cu dissolved in vapor phase in hydrothermal fluids. Experiments prove that Au and Cu can re-distribute in vapor phase and liquid phase during separation of Au- and Cu-bearing supercritical fluids to vapor and liquid phases. These experimental results can illustrate some ore geneses, where boiling phenomena of ore fluids were found. Au- and Cu-bearing NaHCO3-HCl solutions were heated up to more than 350°C in the main vessel, and then passed through a phase separator in a temperature range from 250°C to 300°C, separated into vapor and liquid phases. We collected and analyzed the liquid and vapor samples separately, and found that Au and Cu dissolved and distributed in vapor phase. In some cases, the concentrations of Au and Cu in vapor are higher than those in liquid phase. Those experiments are used to interpret field observations of fluid inclusion data of some Au and Cu deposits, and demonstrate that some Au and Cu ore deposits are derived from metals transportation in vapor phase.