This work and the companion papers discussed at the current MSCMP, 2006, 2010 Nanotech , 2005-2010 TMS and MS&T Conferences continue our efforts to advance GaP/ polymer nanocomposites for light emissive devices based on GaP nanoparticles. The work is prepared in framework of the mentioned below current US/Italy/France/Romania/Moldova project. The components of these nanocomposites demonstrate complementary behavior and each is a candidate for use in light emitters, waveguides, converters, accumulators and other planar, fiber or discrete micro-optic elements. While bulk and thin GaP films have been successfully commercialized for many years, its application in device nanocomposite structures for accumulation, conversion and transport of light energy has only received attention recently. Nanoparticles of GaP have been prepared using yellow P and a mild aqueous low temperature synthesis followed by ultrasonication. The details of preparation of the suitable for light emissive nanocomposites GaP nanoparticles as well as the influence of different temperatures, modifications and compositions of the reacting components on quality of the particles can be found in the papers presented at the current MSCMP. In preparation of the nanocomposite we used the fractions of uniform GaP nanoparticles having after a thorough ultrasonic treatment and a number of other operations improving the quality of the nano-suspension a bright luminescence at room temperature in a broad band with the maximum, dependently on the concrete synthesis conditions, between 2.4 – 3.2 eV, while the value of the forbidden gap in GaP at room temperature is only 2.24 eV. Polyglycidyl methacrylate (PGMA), polyglycidyl methacrylate-copolyoligoethyleneglycol methacrylate (PGMA-co-POEGMA) and biphenyl vinyl ether (BPVE) polymers were used for preparation on GaP nanocomposites. Thickness of the polymer composite film was within 250-300 nm defined from AFM scratch experiment. Surface morphology of the films was studied with AFM. We used the tapping mode to study the surface morphology of the composite films in ambient air. Luminescence of the nanocomposites was excited by the N2 laser nanosecond pulses at wavelength 337 nm and measured at room temperature. We show that thoroughly washed, ultrasonicated and dried nanopowder obtained by mild low temperature aqueous synthesis from yellow P may be used for fabrication of quite good blue light emissive nanocomposite, but the best quality can be obtained only in fabrication of the nanocomposite from similarly prepared nanoparticles, but stored as a suspension in a suitable liquid. So, we demonstrate spectra of luminescence from GaP/ polymer nanocomposites with the pronounced quantum confinement effect and note that the maximum UV shift of the luminescence, app. 1 eV from the position of the forbidden gap in GaP at room temperature, has the nanocomposite prepared on the base of the suspension. Note that our first attempts to prepare GaP nanoparticles, dated by the years 2005-2006 [3], gave their room temperature luminescence with maximum shifted only to 2.4 eV that in comparison with the new maximum at 3.2 eV confirms serious achievements in technology of GaP nanoparticles and GaP based nanocomposites. Recently started investigation of the GaP/BPVE nanocomposite as a prospective light emissive device structure shows that in this nanocomposite the position of the luminescent maximum can be changed between 2.5 – 3.2 eV and the brightness is 20-30 more than in the PGMA and PGMA-co-POEGMA matrixes. Thus, using an improved technology for preparation of GaP nanoparticles and methods of fabrication of the GaP/ polymer nanocomposites we can change within the broad limits the main parameters of their luminescence. The authors are very grateful to the US Department of State, Institute of International Exchange, Washington, DC, Science & Technology Center in Ukraine (STCU) and the US sponsors of the current STCU Project 4610 “Advanced Light Emissive Device Structures”, Clemson University, SC, Institute of Applied Physics and Academy of Sciences of Moldova for support and attention to this research.