Abstract: Provided is a preparation method and use method of a material for deep purification of HF electronic gas. A metal fluoride-loaded activated carbon material AC/MFx.nH20 is prepared, and a mixed gas flow of carbonyl fluoride and high-purity nitrogen is used to deeply dehydrate the material to obtain the material for deep purification of HF electronic gas AC/MFx. This kind of material has fluoride that can form crystal water to form hydrated metal fluoride, and has strong water absorption properties. Moreover, the anhydrous fluoride and activated carbon do not have to face the problem of being corroded by HF, and the collapse of framework structure and the secondary pollution to HF from reaction products would not be caused. The material has the advantages of high purity and extremely low moisture content when being used for efficiently removing moisture in HF.