This　research　focused　on　the　synthesis　of　ultrafine　Ni-Co　composite　powder　prepared　using　a　freeze-drying　technique.　In　the　process　of　freeze-drying,　the　Ni-Co　powder　was　prepared　by　freeze-drying　the　precursor　from　simple　NiC2O4　and　CoC2O4　powders.　Thermal　decomposition　of　the　amorphous　freeze-dried　precursor　powder　produced　the　ultrafine　Ni-Co　composite　powder.　To　assure　process　control　and　product　characterization,　the　freeze-dried　precursor　and　the　final　products　were　analyzed　by　means　of　XRD,　SEM,　TEM,　and　IR.　The　results　showed　that　the　freeze-dried　powder　existed　in　a　non-hygroscopic　and　non-crystalline　state.　The　final　product　of　the　experiments　was　a　Ni-Co　composite　powder,　which　existed　in　the　form　of　a　single　crystalline　state　and　represented　fine,　homogeneous,　spherical　particles,　reaching　a　size　range　of　approximately　40-70　nm.　ne　freeze-dried　powder　was　composed　of　[Ni(NH3)(6)](2+)　and　[Co(NH3)(6)](3+).　(C)　2007　Elsevier　B.V.　All　rights　reserved.