Nanoparticles precipitative synthesis

The major advantage of precipitation synthesis such as the type described above is that large quantities of nanoparticles can be made. However, it can be difficult to tailor the size since only kinetic factors are available to arrest growth. The addition of complexing agents or surfactants can help control particle size. Following the example of gold nanoparticles, it is possible to synthesized... 

This method has been successfully applied for the synthesis of metals, metal oxides, alloys and core-shell nanoparticles. The synthesis of metal oxides from reverse micelles is similar in most aspects to their synthesis in aqueous phase by a precipitation process. For example, precipitation of hydroxides is obtained by addition of a base such as NH3(aq) or NaOH to a reverse micelle solution... 

CuNPs) in Fig. 7 shows the monodisperse and uniformly distributed spherical particles of 10+5 nm diameter. The solution containing nanoparticles of silver was found to be transparent and stable for 6 months with no significant change in the surface plasmon and average particle size. However, in the absence of starch, the nanoparticles formed were observed to be immediately aggregated into black precipitate. The hydroxyl groups of the starch polymer act as passivation contacts for the stabilization of the metallic nanoparticles in the aqueous solution. The method can be extended for synthesis of various other metallic and bimetallic particles as well. 

The synthetic approach is very simple and does not require any special set up. In a typical room temperature reaction, 1.0 mL aqueous solution of cadmium chloride was added to 20 mL aqueous solution of soluble starch in a 50 mL one-necked round-bottom flask with constant stirring at room temperature. The pH of the solution was adjusted from 6 to 11 using 0.1 M ammonia solution. This was followed by a slow addition of 1.0 mL colourless selenide ion stock solution. The mixture was further stirred for 2 h and aged for 18 h. The resultant solution was filtered and extracted with acetone to obtain a red precipitate of CdSe nanoaprticles. The precipitate was washed several times and dried at room temperature to give a material which readily dispersed in water. The same procedure was repeated for the synthesis of PVA and PVP - capped CdSe nanoparticles by replacing the starch solution with the PVA and PVP polymers while the synthesis of elongated nanoparticles was achieved by changing the Cd Se precursor ratio from 1 1 to 1 2. The synthesis of polymer capped ZnSe nanoparticles also follows the same procedure except that ZnCb solution was used instead of CdCb solution. 

The most intensive development of the nanoparticle area concerns the synthesis of metal particles for applications in physics or in micro/nano-electronics generally. Besides the use of physical techniques such as atom evaporation, synthetic techniques based on salt reduction or compound precipitation (oxides, sulfides, selenides, etc.) have been developed, and associated, in general, to a kinetic control of the reaction using high temperatures, slow addition of reactants, or use of micelles as nanoreactors [15-20]. Organometallic compounds have also previously been used as material precursors in high temperature decomposition processes, for example in chemical vapor deposition [21]. Metal carbonyls have been widely used as precursors of metals either in the gas phase (OMCVD for the deposition of films or nanoparticles) or in solution for the synthesis after thermal treatment [22], UV irradiation or sonolysis [23,24] of fine powders or metal nanoparticles. 

Scheme 1 Illustration of the general synthetic method followed in our group for the synthesis of metal nanoparticles i decomposition of the precimsor, nucleation ii first growth process in ripening or coalescence leading to size and shape controlled objects through addition of stabilizers which prevent the full precipitation of the metal (iv)...

The acidic conditions of standard SBA-15 synthesis [35] cause the precipitation of metal nanoparticles without silica encapsulation, or the formation of amorphous silica due to the presence of the polymer used for nanoparticle synthesis. Therefore, the SBA-15 framework was synthesized under neutral condition using sodium fluoride as a hydrolysis catalyst and tetramethylorthosilicate (TMOS) as the silica precursor. Pt particles with different sizes were dispersed in the aqueous template polymer solution sodium fluoride and TMOS were added to the reaction mixture. The slurry aged at 313 K for a day, followed by an additional day at 373 K. Pt(X)/SBA-15-NE (X = 1.7, 2.9, 3.6, and 7.1nm) catalysts were obtained by ex-situ calcination (see Section 3.2). TEM images of the ordered... 

The synthesis of C S-Au nanoparticles as a source for the heat treatment followed the Ernst s two-phase (toluene/water) reaction procedure [3]. The organic (toluene) phase was then separated, evaporated completely in a rotary evaporator at 40 °C, and dried in vacuo at 30 °C for a day. The crude solid obtained was heat treated at 150-250 °C at the heating rate of 2°Cmin, and held for 30 min. The heat-treated product was dissolved in toluene and mixed with methanol to remove excess free C12SH and TOAB. The dark brown precipitate... 

Abstract This chapter discusses the effect of ultrasound propagation in water and aqueous solutions, in the atmosphere of inert and reactive gases. Sonochemical studies of aqueous solutions of divalent and trivalent metal ions and their salts have been reviewed and the precipitation behaviour of hydroxides of metal ions has been discussed. Synthesis of nanoparticles of many metals using ultrasound and in aqueous solutions has also been discussed briefly. Besides, the nephelometric and conductometric studies of sonicated solutions of these metal ions have been reported. 

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