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Research Papers

High Production Rate Synthesis of CdS Nanoparticles Using a Reverse Oscillatory Flow Method

[+] Author and Article Information
Daniel A. Peterson

Mem. ASME
School of Mechanical, Industrial,
and Manufacturing Engineering,
Oregon State University,
Microproducts Breakthrough Institute,
1110 NE Circle Boulevard,
Corvallis, OR 97331
e-mail: dpeterso@engr.orst.edu

C. Padmavathi

School of Mechanical, Industrial,
and Manufacturing Engineering,
Oregon State University,
Microproducts Breakthrough Institute,
1110 NE Circle Boulevard,
Corvallis, OR 97331

Brian K. Paul

Mem. ASME
School of Mechanical, Industrial,
and Manufacturing Engineering,
Oregon State University,
Microproducts Breakthrough Institute,
1110 NE Circle Boulevard,
Corvallis, OR 97331
e-mail: brian.paul@oregonstate.edu

1Corresponding author.

Contributed by the Manufacturing Engineering Division of ASME for publication in the JOURNAL OF MICRO- AND NANO-MANUFACTURING. Manuscript received March 18, 2014; final manuscript received May 20, 2014; published online July 8, 2014. Assoc. Editor: Chengying Xu.

J. Micro Nano-Manuf 2(3), 031004 (Jul 08, 2014) (8 pages) Paper No: JMNM-14-1016; doi: 10.1115/1.4027740 History: Received March 18, 2014; Revised May 20, 2014

A reverse oscillatory flow (ROF) mixing system is discussed having a reaction channel 460 μm high by 152 mm wide for high flow rate processing of nanoparticle (NP) chemistries. The ROF system is demonstrated to produce CdS nanoparticles at a production rate of 115.7 g/h with a coefficient of variation (CV) for particle size down to 19%. These production rates are substantially higher than those achieved using other microchannel mixers while maintaining comparable size distributions. Advantages of the ROF approach include the use of larger microchannels which make the reactor easier to fabricate and less vulnerable to clogging.

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Figures

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Fig. 1

Schematic of a LaMer process showing (1) reagent mixing, (2) particle nucleation, and (3) growth phases

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Fig. 2

CFD rendering of mixing characteristics showing the formation and diffusion of plugs. The contour denotes the species concentration. Image taken from case 12.11 (see Table 3).

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Fig. 3

Schematic of ROF system. The two pumps are 180 deg out of phase which promote mixing within the micromixer. Cuvette is shown which allows for sample collection for UV–Vis, TEM analysis.

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Fig. 4

Experimental facility, including reagent reservoirs, pumps, and micromixer

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Fig. 5

Microreactor schematic with terminology

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Fig. 6

Magnified image of micromixer, showing a realized channel height of 454 μm which is within 2% of the desired height of 460 μm

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Fig. 7

TEM image of CdS NPs synthesized using Case 12.22 and prepared by (a) dispensing a drop on carbon film, (b) dispensing a drop on carbon film and washed with menthol, (c) dispensing a drop of methanol suspension on carbon film, and (d) dispensing a drop on formvar film

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Fig. 8

Concentration contour plot of reagents for (a) case 12.11 and (b) case 30.22

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Fig. 9

TEM and histograms of CdS NPs synthesized using ROF method for variety of operating conditions: (a) case 12.11, PD = 3.8 nm, σ = 1.0 nm, CV = 26.6%; (b) case 18.11, PD = 4.6 nm, σ = 1.1 nm, CV = 23.2%; (c) case 18.22, PD = 7.0 nm, σ = 1.9 nm, CV = 26.9%; and (d) case 12.22H, PD = 6.0 nm, σ = 1.1 nm, CV = 19.0%

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Fig. 10

HRTEM micrographs of CdS NPs obtained at 30.22 with 0.004 M

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Fig. 11

UV–visible absorbance spectra of as-synthesized CdS NPs showing the (a) effect of pump frequency, (b) effect of pump displacement, and (c) effect of concentration

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