A kind of novel magnetic fluorescent hollow nanoparticles with multi-layer shells by layer-by-layer self-assembly process was presented in this paper. Non-crosslinking poly(acrylic acid) (PAA) nanoparticles as core with 250 nm in diameters were prepared by distillation-precipitation polymerization in acetonitrile with 2, 2'-Azobisisobutyronitrile (AIBN) as initiator and without any stabilizer and crosslinker. Then 4-vinylpyridine (4-VPy) as monomer was selfassembled on the surface of PAA nanoparticles because of hydrogen-bonding effect between the surface carboxyl of PAA nanoparticles and pyridine of 4-VPy. The 4-VPy as first shell layer were crosslinked by ethylene glycol dimethacrylate (EGDMA) by seeds distillation-precipitation polymerization in acetonitrile. The core/shell structure of this kind of nanoparticles was investigated by FT-IR and TEM. We can find that the products had an absorption peak at 1641 cm-1 from the FT-IR, which showed that the vinyl groups had been connected in the polyAA microspheres. After that, the non-crosslinking PAA core was removed under a solution of sodium hydroxide in ethanol-water. On the other hand, CdTe quantum dots (QDs) with about 3 nm in diameters as shell were prepared in aqueous solution with 3- mercaptopropionic acid (MPA) as stabilizer and 1, 6-hexylenediamime modified Fe3O4 nanoparticles with about 11 nm in diameters as core were synthesized in water respectively. Because of the hydrogen-bonding between the surface carboxyl of MPA on CdTe QDs and the amino on Fe3O4 nanoparticles, the core/shell magnetic-fluorescent nanoparticles were obtained. Then, the magnetic-fluorescent nanoparticles as second shell layer were self-assembled on the hollow 4VPy nanoparticles.
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