Metallophthalocyanines　(MPc)　have　excellent　photoelectricity　properties.　But　their　low　solubility　in　sol-gel　precursor　and　the　tendency　to　aggregate　make　it　difficult　to　get　their　homogeneously　composites　with　traditional　Sol-gel　schedule.　To　overcome　this　problem,　a　newly　developed　＂in-situ　synthesis＂　technique　during　sol-gel　process　is　successfully　used　to　synthesize　Nickel　phthalocyanine　(NiPc)　in　silica　xerogel　matrix　under　the　irradiation　of　microwave.　As　the　result,　a　new　kind　of　organic/inorganic　nanocomposite　was　obtained.　The　characterization　of　the　glass　sample　and　its　extract　were　carried　out　by　methods　of　IR　and　UV/VIS　spectra.　The　＂in-situ　synthesis＂　mechanism　of　NiPc　and　its　reaction　dynamics　under　the　irradiation　of　microwave　were　discussed.