Continuous Production of Metal Nanoparticles Everett Carpenter VCU John Monnier USC Frank Gupton VCU Center for Rational Catalyst Synthesis University of South Carolina, Columbia, SC June 2014

Research Team: Everett Carpenter, John Monnier, B. Frank Gupton Overview: Utilize c ontinuous reactor technology for the production of metal nanoparticles in order to increase both the quantity and quality of these materials. Continuous Production of Metal Nanoparticles With and Without Microwave Irradiation Technical Information: We will use continuous processing methods to explore the ability to produce to produce bimetallic materials from Group IB (Cu, Ag and Au) and Group VIII (Pd and Pt) metal salts.

Industrial Relevance Although a significant effort has been made in the characterization and application of these materials, viable commercial manufacturing methods for these materials remain a challenge. The manufacturing processes for the production of metal nanoparticles typically employs a batch processing strategy in which metal salts are chemically reduced to produce the metal nanoparticles. There are several drawbacks with this approach which include: Batch to batch variability of physical properties and performance Inability to produce large quantities of material Uncontrolled nucleation on heat transfer surfaces Lack of control of critical process parameters These barriers are further enhanced by using conventional heating techniques that may pose hazardous environmental and working conditions. Such issues are significant to the commercial production and therefore availability of metal nanoparticles for industrial applications.

Goals of the Proposal Use continuous reactor system to explore the ability to produce bimetallic materials from Group IB (Cu, Ag and Au) and Group VIII (Pd and Pt) metal salts. We anticipate that this approach will:  Achieve better control of metal nanoparticles physical properties  Increase throughput of metal nanoparticle manufacturing  Improve safety of and reduce exposure to nanomaterials

Proposed Hypothesis Continuous reactor technology can be applied to the production of metal nanoparticles with and without the use of microwaves, which will provide a reproducible source of materials that can be effectively controlled to meet specific application requirements.

Research Methods/ Techniques  Evaluate the effect of heating and flow rate on particle size distribution -Factorial design of experiments -Conventional Heating vs Microwave  Determine valence state, metal dispersion and particle size distribution  Measure exposed metal sites of bimetallic materials by CO adsorption

Outcomes/ Deliverables  Successful demonstration of continuous production of metal nanoparticles  Control and characterization of particle size and dispersion bimetallic species  CO adsorption in EtOH, H 2 O, and EtOH/H 2 O mixtures on metal nanoparticles  Measurement of adsorption behavior (including competitive adsorption) at different concentrations and temperatures in order to develop mechanistic models for these processes

Impact  Demonstration of method for continuous production of metal nanomaterials  Evaluation and charactorization of bimetallic materials from Group IB (Cu, Ag and Au) and Group VIII (Pd and Pt) metal salt.  Measurment of the exposed metal sites of the bimetallic materials by CO adsorption Duration of Project and Proposed Budget  Two Years  $60,000 Year 1  $60,000 Year 2