Nanopowder　of　rare　earth　tungsten　for　emission　materials　was　prepared　by　freeze-drying　process.　The　solution　of　ammonium　metatungstate　with　rare　earth　nitrate　was　quench-frozen　and　dried　in　vacuum　to　produce　the　mixture　of　ammonium　metatungstate　and　rare　earth　nitrate　powder　with　high　purity.　Most　of　the　powder　existed　in　non-hygroscopic　and　non-crystalline　state.　During　the　experiment,　the　advantage　of　freeze-drying　process　was　successfully　achieved.　High　speed　freezing　also　fixed　the　ion　distribution　that　once　formed　in　the　solution.　Due　to　less　atomic　moves　during　the　subsequent　sublimation　process,　the　homogeneity　of　the　original　solution　was　retained.　The　freeze-dried　compound,　which　consisted　of　ammonium　metatungstate　and　rare　earth　nitrate,　was　reduced　under　various　conditions　to　determine　the　effect　of　reaction　conditions　(temperature　and　time)　on　the　particle　size　of　the　final　rare　earth　tungsten　powder.　Experiments　showed　that　the　grain　size　of　the　powder　mixture　depended　on　the　temperature　and　duration　of　the　reduction　process.　The　characterization　of　the　powder　mixture,　microcompact　and　pellets　were　analyzed　by　means　of　XRD,　FESEM　and　TEM　throughout　the　whole　experimental　process.　(C)　2005　Elsevier　Ltd.　All　rights　reserved.