Synthesis and characterization of silver nanoparticles by sonoelectrodeposition

Shaped silver nanoparticles with sphere, wire and dendrite were prepared by sonoelectrochemical deposition from an aqueous solution of AgNO3 in the presence of ethylenediaminetetraacetic acid disodium salt （EDTA） and polyvinylpyrrolidone （PVP）. The diameter of spherical silver particles was about 30 nm. The diameter of the silver nanowires was also about 30 nm and the length was 200-900 nm. The dendrites were synthesized with the concentration of silver solution increasing. Silver nanoparticles were characterized by transmission electron microscope （TEM）, X-ray powder diffraction （XRD）, scanning probe microscope （SPM） and UV-vis absorption spectrum. XRD patterns revealed that silver particles were of face-centered cubic structure. UV-vis absorption spectra indicated that different morphology and size of silver particles could influence the optical properties.     

Synthesis and characterization of metallic Pd embedded TiO2 nanoparticles by reverse micelle and sol-gel processing

This research was financially supported by the Ministry of Education, Science Technology(MEST) and Korea Industrial Technology Foundation(KOTEF) through the Human Resource Training Project for Regional Innovation.     

溶剂热法Fe3O4纳米颗粒的制备及表征

以乙醇及水的混和溶剂、单质Fe为原料在高温高压反应釜中制备了Fe3O4纳米颗粒。XRD及红外分析表明所获得产物为Fe3O4。高分辨透射电镜观察表明,Fe3O4具有长棒状形貌,长度为200～500nm,直径为20～30nm。所获得Fe3O4纳米颗粒具有良好的铁磁性能,其饱和磁化强度达到64.75emu/g。讨论了Fe3O4纳米颗粒的形成机制。     

Synthesis of ZnS nanoparticles via hydrothermal process assisted by microemulsion technique

Uniform and spherical ZnS nanoparticles with a diameter of 5–10 nm were successfully synthesized at 160 °C via a facile hydrothermal process, where ZnS precursors were prepared by a microemulsion technique. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescent (PL) spectra techniques, respectively. The results showed that the hydrothermal temperature exerted a more important effect than the holding time on the crystallization of ZnS crystallites. The as-prepared ZnS nanoparticles exhibited higher PL intensity than that of the normal ones of micrometer scale besides an obvious blue shift.     

机械化学法制备氮化硼纳米管及纳米粒子

通过高能球磨及随后的退火过程,在同一实验参数下制备了氮化硼纳米管和纳米粒子.制备的氮化硼纳米管呈竹节状,直径为20～100 nm,长度约为几个微米.制备的氮化硼纳米粒子尺寸均匀,大部分呈圆片状,少数为球状;直径为20～100nm,多数粒子直径为70 nm.同一制备参数下形成不同形态氮化硼纳米材料的原因在于氮化硼米管及纳米粒子的形成机理不同.     

One-step reverse micelle polymerization of organic dispersible polyaniline nanoparticles

Organic solvent dispersible dodecylbenzenesulfonic acid (DBSA)-doped polyaniline (PANI) was prepared from DBSA micelles with ammonium persulfate (APS) as an oxidant in hexane by one-step polymerization. Morphology observation showed PANI–DBSA powder polymerized with 0.0375 mol DBSA consisting of spherical particles having diameters of 40–60 nm that formed irregular aggregates with about 1 μm diameter. Polymerization was carried out in the hydrophilic aqueous microdomains of micelle dissolved reactants. The experimental conditions were optimized for direct synthesis of DBSA-doped PANI with high electrical conductivity by adjusting various reaction conditions. This research showed the importance of adjusting reaction conditions such as DBSA, aniline, ammonium persulfate, and acidity for polymerization. It was also found that a portion of an electrically neutral anilinium–DBSA complex could be assembled into reverse micelles together with DBSA molecules, where DBSA and anilinium–DBSA acted as both surfactants and doping agents to achieve nano-scaled DBSA-doped PANI with high conductivity. The doping level of DBSA in PANI particles was studied by UV–vis spectroscopy and X-ray diffraction (XRD). From TG/DTA/mass spectrometry, it was found that the PANI–DBSA was doped with both free and bound DBSA.     

Solvent effects in the synthesis of MgFe2O4 nanopowders by reverse micelle processing

Nanopowders of MgFe₂O₄ have been synthesized by the novel and facile reverse microemulsion route. The effects of changing the continuous phase on the particle size and the magnetic property have been studied. The average particle size, morphology and saturation magnetization are shown to be dependent on the continuous phase. The average diameters of the particle prepared with heptane are 20.9 ± 4.3 nm. On the contrary, the product with toluene and cyclohexane is highly aggregated. The values of saturation magnetization for our samples prepared with heptane, toluene and cyclohexane are 14.5, 30 and 37 emu/g.     

Synthesis of high-purity silver colloids using a thermal decomposition method

A thermal decomposition method was employed to produce high purity Ag particles. Silver carbonate was dispersed in an H₂O solvent that was heated above 80°C, followed by rapidly injecting H₂O₂ into the solvent. Then, the silver carbonate was decomposed into nanosized Ag particles using the decomposition heat of hydrogen peroxide as follows: Ag₂CO₃→2Ag+CO₂+1/2O₂. The size of the synthesized Ag particles is approximately 100 nm. This method can be used to produce high-purity Ag colloids withuut impurities, unlike other methods.     

Synthesis of Ag/SiO2 nanosize particles by reverse micelle and sol-gel processing

Ag/SiO₂ composite particles have been synthesized within reverse micelle via metal alkoxide hydrolysis and condensation. The size of the particles and the thickness of the coating can be controlled by manipulating the relative rates of the hydrolysis and condensation reactions of tetraethoxysilane (TEOS) within the microemulsion. The average size of the synthesized particles was in the size range of 20–40 nm. The effects of synthesis parameters, such as the concentration of the Ag solution, the molar ratio of water to TEOS, and the molar ratio of water to surfactant, are discussed.     

溶液法和反胶束法制备Fe-B颗粒的结构和磁性能

采用溶液法和反胶束法合成Fe-B磁性纳米颗粒.通过XRD、TEM、ICP、VSM等手段,依次对Fe-B纳米颗粒的结构、形貌、成分、磁性能进行表征,并针对两种方法所得结果进行对比分析.采用溶液法制备的Fe-B纳米颗粒为晶体结构,颗粒尺寸在20~70 nm;反胶束法合成的Fe-B磁性纳米颗粒一般为非晶结构,颗粒尺寸细小(约5 nm).ICP颗粒成分分析结果表明,两种方法制备的Fe-B颗粒中B含量不同,溶液法制备的Fe-B颗粒中B含量约为17.8 at%;而反胶束法制备的Fe-B颗粒,其B含量较高,达34.9 at%.上述结构、颗粒尺寸和B含量的差异,导致了两种方法合成的Fe-B颗粒在磁性能方面的差别.     

AOT reverse micelle, a new organized medium for the electrosynthesis of polyaromatic hydrocarbons; application to the electropolymerization of biphenyl

Electrosynthesis of poly(biphenyl) (PBP) films was performed in an AOT [sodium bis(2-ethylhexyl) sulfosuccinate] reverse micelle by cyclic voltammetry and chronopotentiometry on a platinum electrode. An electroactive PBP film was formed either by cyclic voltammetry between −0.6 and 1.65 V/Ag/AgCl or under current control (j = 0.2 mA/cm²). PBP films were characterized electrochemically and spectroscopically (MALDI-TOF mass spectrometry), NMR, Raman, FT-IR, X-ray photoelectron and UV–vis spectroscopy). The structure of the PBP films involved sequences of ramified trimer possessing quinoid forms. This type of sequences can give strongly condensed oligomers with PBP molar mass up to 2669.6 g/mol according to the electrosynthesis charge.     

Preparation and formation mechanism of Al2O3 nanoparticles by reverse microemulsion

Al2O3 nanoparticles were prepared by polyethylene glycol octylphenyl ether（Triton X-100）/n-butyl alcohol/cyclohexane/ water W/O reverse microemulsion. The proper calcination temperature was determined at 1 150 ℃ by thermal analysis of the precursor products. The structures and morphologies of Al2O3 nanoparticles were characterized by X-ray diffraction, transmission electron microscopy and UV-Vis spectra. The influences of mole ratio of water to surfactant on the morphologies and the sizes of the Al2O3 nanoparticles were studied. With the increase of surfactant content, the particles size becomes larger. The agglomeration of nanoparticles was solved successfully. And the formation mechanisms of Al2O3 nanoparticles in the reverse microemulsion were also discussed.     

Synthesis and characterization of Ba(CoxNb1-x)O3 nanoparticles by hydrothermal processing

The nanosized Ba(Co_xNb_1–x)O₃(BCN) particles were prepared under high temperature and pressure conditions by precipitation from metal nitrates with aqueous potassium hydroxide. Ba(Co_xNb_1–x)O₃ powders were obtained in the temperature range of 170–210 °C for 6 h. The results show that the average size of the synthesized particles increases with increasing reaction temperature. The average size of the synthesized particles is about 10 nm. The crystalline phase of the synthesized particles is found to be Ba(Co_xNb_1–x)O_3. Ceramics derived from the nano BCN powders could achieve high sintering density at a relatively low sintering temperature.     

球形纳米银粉体制备及其表征

采用均匀沉淀和高温热分解相结合的方法制备了纳米银粉体,分析了纳米银粉体形成机理,研究了初始浓度、烧结温度和时间对纳米银粉体粒径和形貌的影响;采用X射线衍射仪、扫描电子显微镜表征了纳米银粉体结构、组成、大小和形貌。结果表明,硝酸银初始浓度0.05 mol/L、烧结温度300℃、烧结2 h,以尿素为pH控制剂,不添加任何其他分散剂条件下可得到分散性好、颗粒均匀,粒径50 nm的球形粉体。     

Preparation of nanostructure silver powders by mechanical decomposing and mechanochemical reduction of silver oxide

The mechanical decomposing and mechanochemical reductions of silver oxide for preparation of nanocrystalline silver powders by high planetary ball mill was investigated. XRD and HRSEM techniques were used to characterize the structural evolution and morphological changes of products. The results show that the nanostructured silver with an average crystallite size of 14 nm and internal strain of 0.75% is synthesized by mechanical decomposing of Ag₂O after 95 h milling. While, the product of mechanochemical reduction of silver oxide using graphite after 22 h milling is nanostructured silver with an average crystallite size of 28 nm and internal strain of 0.44%.     

Synthesis and magnetic properties of CoPt nanoparticles

CoPt nanoparticles were prepared by simultaneous thermally reducing Co(CH3COO)2 and Pt(acac)2 in oleylamine with a small quantity of oleic acid. The composition of the particles was controlled by changing the amount of the reactants. Transmission electronic microscopy reveals that Co 48 Pt 52 particles with an average diameter of 8.4 nm are steadily dispersed in octane in the presence of oleylamine and oleic acid. Selected area electron diffraction indicates that the as-prepared particles have a face center cubic structure. Magnetic properties of these particles measured by a vibrate sample magnetometer yield a coercivity of 1.194×104 A·m-1 and a saturation magnetization of 5.3 emu·g-1 . After annealing at 650 ℃ for 2 h under the flowing Ar, the coercivity increases to 9.552×104 A·m-1 according to partly phase transformation from face center cubic structure to face center tetragonal structure for the nanoparticles.     

水热法批量制备粒径可控SnO2纳米粉体（英文）

以SnCl4·5H2O为前驱体、NH3·H2O为矿化剂,通过水热还原技术制备平均粒径在5～30nm的SnO2纳米粉末。系统研究小批量生产(1kg/批)条件下,工艺条件包括溶液浓度、反应温度、压力、时间和pH值对SnO2粒径、形貌和晶型的影响,并采用XRD、TEM等测试手段对样品进行表征。结果表明,在保持SnO2粉末晶型和形貌不变的前提下,通过调节反应温度、反应时间等工艺参数,粉末的粒径尺寸可以有效地控制在5～30nm范围内。不同于之前的报道,SnO2粒径尺寸随着反应时间(反应温度)的变化存在新的变化趋势,并推测解释了此晶粒异常生长的机理。     

Double reverse flotation process of collophanite and regulating froth action

A new double reverse flotation process was used to beneficiate the Yichang region collophanite of Hubei Province, China. Its final concentrate yield is 67.37%, P2O5 grade is 32.17%, P2O5 recovery is 87.80%, and the main impurities MgO, Fe203 and Al2O3 are 0.95%, 1.04%, 1.36%, respectively. The difficult problem was successfully solved that plentiful froths are bought by the cationic collector reverse flotation in collophanite beneficiation by adding inorganic froth regulator CA to the pulp. The defrothing mechanism was studied through mensurating surface tension and Zeta potential of the pulp after adding CA. It is found that the changing of surface tension and hoisting of Zeta potential may be the main reasons that froths become friable and break up.     

Synthesis and characterization of aminated SiO2/CoFe2O4 nanoparticles

A kind of newly aminated CoFe2O4 nanoparticles were synthesized by grafting process for biomedical applications, which were coated primarily with silicon dioxide（SiO2）. The characterizations of aminated SiO2/CoFe2O4（ASCN） and SiO2-coated CoFe2O4（SCN） nanoparticles were investigated using elemental analysis, thermogravimetric analysis（TGA）, differential thermal analysis（DTA）, infi＇ared spectroscopy（IR）, atomic force microscopy（AFM）, zeta-potential measurement and vibrating sample magneto-metry（VSM） The AFM micrograph shows that the ASCN nanoparticles are approximately spherical with an average diameter of 30 nm. Based on IR and TGA results, it is suggested that the surface of the SiO2-coated CoFe2O4 nanoparticles are graiied with amino compounds. The elemental analysis also shows the presence of 0.98 mmol/g of organic moieties immobilized on the surface ofASCN nanoparticles. Zeta-potential data ofASCN nanoparticles also reveal that amino compounds are bonded onto the surface of SiO2-coated CoFe2O4 nanoparticles by ether linkage. The magnetic parameters show that ASCN nanoparticles still have good magnetic property.     

Synthesis of nanoparticles of silver and platinum by microwave-induced plasma in liquid

We have conducted a basic study of microwave plasma in liquid at atmospheric pressure. Plasma could be successfully induced by radiated microwave from pointed and ring tungsten electrodes. The tungsten electrode showed a long lifetime of 70 h. Melting and chemical etching of the electrode's top limited the lifetime. Silver cations from silver nitrates could be rapidly and completely reduced to generate metallic silver nanoparticles using this plasma source without any addition of reducing chemical reagents. Optimization of electric conductivity of the reaction solution was not needed. When the material of the electrode was changed to platinum from tungsten, platinum nanoparticles were produced by vaporization into pure water. Both these preparation processes can be expected to produce lower contamination than chemical synthesis.