The stability and spatial separation of nanoparticles (NPs) is essential for employing their advantageous nanoscale properties. This work demonstrates the entrapment of gold NPs embedded in a porous inorganic matrix. Initially, gold NPs are decorated on fibrous nylon-6, which is used as an inexpensive sacrificial template. This is followed by inorganic modification using a novel single exposure cycle vapor phase technique resulting in distributed NPs embedded within a hybrid organic-inorganic matrix. The processing is extended to the synthesis of porous nanoflakes after calcination of the modified nylon-6 yielding a porous metal oxide framework surrounding the disconnected NPs with a surface area of 250 m(2)/g. A unique feature of this work is the use of a transmission electron microscope (TEM) equipped with an in situ annealing sample holder. The apparatus affords the opportunity to explore the underlying nanoscopic stability of NPs embedded in these frameworks in a single step. TEM analysis indicates thermal stability up to 670 degrees C and agglomeration characteristics thereafter. The vapor phase processes developed in this work will facilitate new complex NP/oxide materials useful for catalytic platforms.