Effects　of　preparation　technology　on　structure　and　thermoelectric　properties　of　NixCo4-xSb12　(x=0.1　similar　to　0.5)　(x=0.1　similar　to　0.5)　were　investigated　separately　by　solid　reaction-spark　plasma　sintering　(SR-SPS)　and　mechanical　milling-spark　plasma　sintering　(MG-SPS)　method.　The　two　methods　had　little　effect　on　phase　structure　and　Seebeck　coefficient,　but　SR-SPS　technology　augments　electrical　resistivity　and　the　grain　size　of　products　when　the　content　of　Ni　was　as　low　as　0.1,　and　hence　increase　the　thermal　conductivity　and　decrease　the　thermoelectric　properties.　Compared　with　SR-SPS,　MG-SPS　method　not　only　is　simple　and　convenient　in　preparation,　but　also　is　propitious　to　the　improvement　the　thermoelectric　properties.　In　our　experimental　range,　the　Ni0.2CO3.8Sb12　bulk　sintered　by　MG-SPS　shows　maximum　ZT　value　of　0.6　at　about　773　K.