Synthesis of Hollow Carbon Nano-Onions Using the Pulsed Plasma in Liquid.

We synthesized carbon nano-onions (CNOs) using a low-voltage spark discharge in a liquid and studied the effects of liquid type and pulse duration. By the pulsed electric discharge between two graphite rods of 120 mm length and 6 mm diameter submerged into a 200 ml toluene or ethanol, hollow CNOs with diameters ranging from 10 to 30 nm were produced. CNOs produced using toluene grew more carbon shells than does the sample produced using ethanol. The sample that was synthesized using pulsed plasma with pulse duration of 5 µs showed more carbon shells (10-30) than the sample prepared by 12 µs (2 to 10). High performance liquid chromatography (HPLC) and high resolution transmission electron microscopy analyses confirmed that the sample produced at 12 µs pulsed plasma contains fullerene C60, while the sample prepared at 5 µs does not.

Synthesis of novel CoCx@C nanoparticles.

CoC(x) nanoparticles encapsulated in carbon shells were synthesized using a pulsed plasma in liquid ethanol. This is the first time that monolithic cubic phase cobalt carbide nanoparticles have been obtained. X-ray diffraction refinement of the nanoparticles showed that the lattice parameter of prepared cubic phase cobalt carbide is larger than that of CoC(x) (44-0962) and cubic phase Co (15-0806 and 01-1259). The x-ray absorption fine structure spectra near the Co K-edge of the synthesized sample indicated differences from commercial metallic cobalt and cobalt oxide samples. High resolution transmission electron microscopy revealed that a thin carbon coating covered the surface of the nanoparticles. These carbon layers might isolate core CoC(x) material from the outside environment, and allow functionalization by carboxyl groups for the further purpose of targeted drug delivery. The obtained CoC(x)@C particles, with a crystallite size of about 10 nm confirmed by the electron microscope, aggregate into 20-40 nm secondary particles in distilled water as shown by dynamic light scattering, and possess high saturation magnetization of about 120 emu g(-1). The sodium 3'-[1-(phenylaminocarbonyl)-3,4-tetrazolium]-bis(4-methoxy-6-nitro)benzene sulfonic acid hydrate assay and defragmentation of deoxyribonucleic acid on MCF-7 cells after incubation with particles indicate relatively low cytotoxicity of CoC(x)@C nanoparticles, compared with micro-sized and nano-sized metallic cobalt particles and commonly used iron oxides. For the small sized CoC(x)@C particles, the release of cobalt ions was checked by a chelation method with ethylenediaminetetraacetic acid solution to be at a very low level compared with other reference materials.

Wurtzite-type ZnS nanoparticles by pulsed electric discharge.

The synthesis of wurtzite-type ZnS nanoparticles by an electric discharge submerged in molten sulfur is reported. Using a pulsed plasma between two zinc electrodes of diameter 5 mm in molten sulfur, we have synthesized high-temperature phase (wurtzite-type) ZnS nanocrystals with an average size of about 20 nm. The refined lattice parameters of the synthesized wurtzite-type ZnS nanoparticles were found to be larger than those of the reported ZnS (JCPDS card no 36-1450). Synthesis of ZnMgS (solid solution of ZnS and MgS) was achieved by using ZnMg alloys as both cathode and anode electrodes. UV-visible absorption spectroscopy analysis showed that the absorption peak of the as-prepared ZnS sample (319 nm) displays a blue-shift compared to the bulk ZnS (335 nm). Photoluminescence spectra of the samples revealed peaks at 340, 397, 423, 455 and 471 nm, which were related to excitonic emission and stoichiometric defects.

Synthesis of blue amorphous TiO2 and Ti(n)O(2n-1) by the impulse plasma in liquid.

Synthesis of blue amorphous TiO2 and Ti(n)O(2n-1) by the impulse plasma in dielectric liquid is presented. The impulse plasma in liquid enables us to quench from plasma state, by which we can synthesize nanomaterials, metastable materials, etc. By the impulse plasma between titanium rods submerged into water, we have synthesized blue colored amorphous TiO2 nanoparticles suspended in water and black titanium monoxide at the bottom. Different types of titania oxides like Ti3O, TiO, Ti2O3, Ti4O7 were produced by the impulse plasma in different water temperatures (3, 30, 60, and 90 degrees C respectively). High Resolution Transmission Electron Microscopy analysis showed that the amorphous TiO2 contains anatase nanocrystals with less than 10 nm. UV-vis absorption spectra of the blue TiO2 nanoparticles showed higher absorbance of visible light than the commercially available pure anatase nanoparticles.

Synthesis method of nanomaterials by pulsed plasma in liquid.

A new synthesis method of nanomaterials using pulsed plasma in liquid by the low voltage spark discharge is presented. The fullerene C60 and TiO nanopowder were for the first time synthesized by electric discharge method in liquid. The purity of C60 was >99%, which is much higher than those by the conventional arc plasma in inert gas methods (less than 80% C60 and 20% C70 and other fullerenes). Copper nanoparticles prepared by this method were smaller than those by arc method by a factor of >5. The pulsed plasma in liquid enables us to quench from plasma state, by which we can synthesize nanomaterials, metastable materials, etc. In addition, the applied power is 100 times smaller than those of arc discharge.