Tin antimonide alloy was obtained for the first time using a very simple dry microwave route. Up to 1 g of well crystallized SnSb can be easily prepared in 90 s under air in an open crucible. A full characterization by X-ray diffraction and 119Sn Mössbauer spectroscopy demonstrated the benefit of carbon as susceptor, which avoid any oxide contamination. The microwave-prepared SnSb was tested as negative electrode material in Li batteries. Interesting results in terms of capacity and rate capability were obtained with up to 700 mAh/g sustained after 50 cycles at variable current. These results pave the way for the introduction of microwave synthesis as realistic route for a rapid, low cost and up-scalable production of electrode material for Li batteries or other large scale application types.