Synthesis and characterization of nickel nanoparticles by hydrazine reduction in ethylene glycol

The synthesis of nickel nanoparticles by the hydrazine reduction of nickel chloride in ethylene glycol at 60 degrees C without soluble polymer as a protective agent was studied. It was found that an appropriate amount of NaOH was necessary for the formation of pure nickel nanoparticles. Also, it was not necessary to perform the reaction under a nitrogen atmosphere. By the analyses of X-ray diffraction, high-resolution transmission electron microscopy, and electron diffraction pattern, the resultant particles were characterized to be pure crystalline nickel with a face-centered cubic (fcc) structure. By transmission electron microscopy, it was observed that the mean diameter decreased with increasing the ratio of [N2H5OH]/[NiCl2] and approached a constant when [N2H5OH]/[NiCl2]>12. In addition, the resultant nickel nanoparticles could be magnetically recovered and re-dispersed in ethylene glycol without size change and agglomeration. The magnetic measurements indicated they were superparamagnetic with a saturation magnetization of 22 emu/g, a remanent magnetization of 6.4 emu/g, and a coercivity of 0.1 Oe at a mean diameter of 9.2 nm. Also, the magnetization increased with decreasing temperature due to the decrease in thermal energy. All the observed magnetic properties essentially reflected the nanoparticle nature. Furthermore, it was found that hydrazine was catalytically decomposed to hydrogen and nitrogen gases by the resultant nickel nanoparticles. The corresponding decomposition rate at 25 degrees C and 1 atm was 3.1 nmol/(h mg of Ni).     

A nonviral transfection approach in vitro: the design of a gold nanoparticle vector joint with microelectromechanical systems

Au nanoparticles modified with 21-base thiolated-oligonucleotides have been evaluated as delivery vehicles for the development of a nonviral transfection platform. The electromigration combined with electroporation for DNA delivery in an osteoblast like cell was employed to test on microchips. Electroporation introduces foreign materials into cells by applying impulses of electric field to induce multiple transient pores on the cell membrane through dielectric breakdown of the cell membrane. On the basis of the characteristic surface plasmon of the Au particles, UV-vis absorption was utilized to qualitatively judge the efficiency of delivery. Transmission electron microscopy images and atomic absorption measurements (quantitative analysis) provided evidence of the bare Au and Au/oligonucleotide nanoparticles before and after electroporation and electromigration function.The experiments demonstrated that electrophoretic migration followed by electroporation significantly enhanced the transportation efficiency of the nanoparticle-oligonucleotide complexes as compared with electroporation alone. Most interestingly, Au capped with oligonucleotides led to optimal performance. On the other hand, the bare Au colloidal suspensions resulted in aggregation, which might be an obstacle to the internalization process. In addition, analytical results demonstrated an increase in the local particle concentrations on the cell surface that provided additional support for the mechanism underlying the improved Au nanoparticle transportation into cells in the presence of electromigration function.     

Synthesis of Strontium Ferrite Ultrafine Particles Using Microemulsion Processing

The strontium ferrite ultrafine particles have been prepared using the microemulsion processing. The mixed hydroxide precursor was obtained via the coprecipitation of Sr(2+) and Fe(3+) in a water-in-oil microemulsion of water/CTAB/n-butanol/isooctane. According to the investigation on the thermochemical properties by TGA/DTA and the phase analysis by XRD, it was shown that the precursor could yield pure strontium ferrite after calcination at 700 degrees C for 5 h while using an appropriate molar ratio of Sr/Fe in microemulsions. From TEM measurement, the diameters of the precursor and calcined particles were 3.8+/-0.7 and 50-100 nm, respectively. The magnetic properties characterized by a SQUID magnetometer showed that the saturation magnetization, remanent magnetization, coercivity, and squareness ratio were 55 emu/g, 28 emu/g, 492 Oe, and 0.51, respectively. The magnetization was also observed to increase with the decrease of temperature at 5-400 K. Compared with those reported earlier, the quite low coercivity implies the potential application of final product in the high-density perpendicular recording media. Copyright 2001 Academic Press.     

Cyclodextrin-conjugated nanocarrier for magnetically guided delivery of hydrophobic drugs

A magnetic nanosystem that simultaneously implements the cyclodextrin–drug complexation power, bioadhesive property of gum arabic (GA) and inherent magnetic properties of Fe₃O₄ nanoparticles, has recently been reported. In this study, a magnetic nanocarrier was fabricated by conjugating 2-hydroxypropyl-cyclodextrin (HCD) onto the gum arabic modified magnetic nanoparticles (GAMNP). The analyses of transmission electron microscopy (TEM) and dynamic light scattering (DLS) revealed that the product had a mean diameter of 14.8 nm and a mean hydrodynamic diameter of 29.3 nm. This nanocarrier showed good loading efficiency for ketoprofen. In addition, the in vitro release profile of ketoprofen from HCD-GAMNP was characterized by an initial fast release followed by a delayed release phase. In view of the better biocompatibility and the combined properties like specific targeting, complexation ability with hydrophobic drugs makes the nanosystem an exciting prospect for drug delivery.     

Spontaneous formation of Ag nanoparticles in dimethylacetamide solution of poly(ethylene glycol)

The spontaneous formation of Ag nanoparticles in a dimethylacetamide (DMAC) solution of poly(ethylene glycol) (PEG) was studied. FTIR analysis showed the formation of carbonyl groups, revealing that PEG acted as not only a protective agent but also a reducing agent in the formation of Ag nanoparticles. Since no significant reactions were observed when poly(tetramethylene glycol) (PTMG) was used to replace PEG or acetonitrile was used to replace DMAC, it was suggested that PEG molecules might be coiled to form pseudo-crown ether cavities, in which Ag complexes were bound to the oxyethylene groups and reduced, and that the use of a solvent which might appropriately solvate the Ag salt was important for the formation of Ag nanoparticles. In addition, the mean diameters of the resultant Ag nanoparticles were 3.8-9.0 nm, increasing with increasing AgNO(3) concentration. A sufficiently high PEG concentration relative to AgNO(3) was necessary for the formation of smaller Ag nanoparticles. This work provided a simple route for the in situ synthesis of Ag nanoparticles.     

Preparation and adsorption properties of monodisperse chitosan-bound Fe3O4 magnetic nanoparticles for removal of Cu(II) ions

Monodisperse chitosan-bound Fe(3)O(4) nanoparticles were developed as a novel magnetic nano-adsorbent for the removal of heavy metal ions. Chitosan was first carboxymethylated and then covalently bound on the surface of Fe(3)O(4) nanoparticles via carbodiimide activation. Transmission electron microscopy micrographs showed that the chitosan-bound Fe(3)O(4) nanoparticles were monodisperse and had a mean diameter of 13.5 nm. X-ray diffraction patterns indicated that the magnetic nanoparticles were pure Fe(3)O(4) with a spinel structure, and the binding of chitosan did not result in a phase change. The binding of chitosan was also demonstrated by the measurement of zeta potential, and the weight percentage of chitosan bound to Fe(3)O(4) nanoparticles was estimated to be about 4.92 wt%. The chitosan-bound Fe(3)O(4) nanoparticles were shown to be quite efficient for the removal of Cu(II) ions at pH>2. In particular, the adsorption rate was so fast that the equilibrium was achieved within 1 min due to the absence of internal diffusion resistance. The adsorption data obeyed the Langmuir equation with a maximum adsorption capacity of 21.5 mg g(-1) and a Langmuir adsorption equilibrium constant of 0.0165 L mg(-1). The pH and temperature effects revealed that the adsorption capacity increased significantly with increasing pH at pH 2-5, and the adsorption process was exothermic in nature with an enthalpy change of -6.14 kJ mol(-1) at 300-330 K.     

Ab initio structure study from in-house powder diffraction of a novel ZnS(EN)0.5 structure with layered wurtzite ZnS fragment

The solvothermal reaction of elemental zinc with sulfur in ethylenediamine (en) as solvent yields [ZnS-0.5(NH2CH2CH2NH2)], 1, an unprecedented ethylenediamine pillared ZnS layered compound, containing two dimensional (2-D) boat-type 6-membered rings, which was characterized by ab initio structure solution from powder diffraction data (SDPD).     

Catalyst-free low temperature synthesis of discrete anatase titanium dioxide nanocrystals with highly thermal stability and UVC-cut capability

A novel, facile, catalyst-free, and low temperature process for the synthesis of discrete anatase TiO₂ nanocrystals has been developed in the absence of stabilizing agent. The product was shown to be discrete anatase TiO₂ nanocrystals with a mean diameter of 4.97 ± 0.9 nm and a specific surface area of 393 m²/g. By varying the water content and precursor concentration, the particle size could be tuned. Also, the resultant colloid solution was quite stable even in the absence of stabilizing agent because of the coverage of EG molecules on the particle surface. In addition, the anatase TiO₂ nanocrystals obtained in this work had highly thermal stability even at temperatures up to 800 °C. Also, as compared to Degussa P25 TiO₂ powders, they exhibited stronger absorption at 200–350 nm and higher transmittance in the visible light region. Thus, the new approach proposed in this work was practicable for the synthesis of anatase TiO₂ nanocrystals, particularly for those requested to have highly thermal stability and UVC-cut capability.

     

Synthesis of Barium Ferrite Ultrafine Particles by Coprecipitation in the Presence of Polyacrylic Acid

The barium ferrite ultrafine particles were synthesized by coprecipitation in an aqueous solution with polyacrylic acid (PAA) as a protective agent. Thermal analysis by TGA/DTA showed that the precursor could yield barium ferrite after calcination above 700 degrees C for 2 h. By analyses of the XRD and electron diffraction pattern, the formation of pure barium ferrite was confirmed and the appropriate molar ratio of Ba/Fe in aqueous solution was determined to be 1/11. The TEM measurements indicated that the average diameter of the precursor was 4.5 nm, and the diameters of the particles calcined at 700 and 800 degrees C were 23-34 and 49-82 nm, respectively. The magnetic properties characterized by a SQUID magnetometer showed that the barium ferrite ultrafine particles calcined at 700-800 degrees C had a saturation magnetization of 36.9-60.8 emu/g, a remanent magnetization of 19.0-31.0 emu/g, a coercivity of 117.3-221.8 Oe, and a squareness ratio of 0.51. The magnetization was also observed to increase with a decrease of temperature at 5-400 K. These magnetic properties all reflected the nature of ultrafine particles and also were influenced by the morphology and microstructure of final products. Copyright 2001 Academic Press.     

Synthesis of high-concentration Cu nanoparticles in aqueous CTAB solutions

Pure metallic Cu nanoparticles at a high concentration (up to 0.2 M) have been synthesized by the reduction of cupric chloride with hydrazine in the aqueous CTAB solution. The input of extra inert gases was not necessary. The use of ammonia solution for the adjustment of solution pH up to 10 and the use of hydrazine as a reducing agent in a capped reaction bottle are crucial for the synthesis of pure Cu nanoparticles. The reaction solution finally became wine-reddish and its UV/vis absorption spectrum exhibited an absorption band at 574 nm, revealing the formation of metallic Cu nanoparticles. By the analysis of electron diffraction pattern, EDS, XRD, and XPS, the resultant particles were confirmed to be pure Cu with a face-centered cubic (fcc) structure. From the TEM analysis, it was found that the mean diameter of Cu nanoparticles first decreased and then approached a constant with the increase of hydrazine concentration. In addition, the CTAB concentration had not significant influence on the size of Cu nanoparticles. Also, TG analysis indicated that there were two weight-loss steps for the CTAB-capped Cu nanoparticles. It was suggested that a bilayer structure of CTAB was formed on the surface of Cu nanoparticles to prevent from the particle agglomeration. The synthesis method reported in this work might be helpful for the large-scale production of Cu nanoparticles.