283563 Factorial Experiment Design in Colloid Nanoparticle Synthesis

Monday, October 29, 2012
Hall B (Convention Center )
Cun Wen1, Jason Hattrick-Simpers2 and Jochen Lauterbach2, (1)Department of Chemical Engineering, University of South Carolina, Columbia, SC, (2)Chemical Engineering, University of South Carolina, Columbia, SC

FACTORIAL EXPERIMENT DESIGN IN COLLOID NANOPARTICLE SYNTHESIS

Cun Wen, University of South Carolina, Columbia, SC

Jason Hattrick-Simpers, University of South Carolina, Columbia, SC

Jochen Lauterbach, University of South Carolina, Columbia, SC

Recently, colloid nanoparticle synthesis has emerged as an effective way to tune the morphology, structure, and size of nanoparticles. Colloid nanoparticle synthesis involves multiple operation parameters, such temperature, concentration, reduction agent, and gas environment. These parameters influence the particle morphology and size in different manners and to varying degrees. Together they form a multidimensional parameter space with non-linear interdependencies between the parameter, such a space can be very time consuming to map out and to interpret utilizing traditional experimental design and synthesis protocols.

Herein, we demonstrate the application of factorial experimental design to CoCu colloid core-shell nanoparticle synthesis. With this approach a series of experiments that decouple the influences of 5 parameters in the synthesis procedure were studied. The 5 parameters include reaction temperature, temperature ramping rate, and concentration of the precursors, capping agent, and reductant. Though we swept out a wide parameter space, the core-shell structures of the nanoparticles are maintained. Among the five parameters, we found that the ramping rate and the capping agent concentration are several orders of magnitude more effective in controlling the particle size as compared to the other parameters. One representative contour map based on factorial design is shown in figure 1. The effect of ramping rates and capping agent concentration can be understood to increase the nucleation speed, and thus lead to a reduction in the particle size.

Figure 1. The contour map of the influence of temperature ramping rate and PVP concentration on the particle size.

To summarize up, with the factorial design, the effects and cross-effects of five synthesis parameters are quantitatively described. Furthermore, following predictions from the factorial design, nanoparticles with small sizes were successfully synthesized.


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