DOI: 10.1126/science.280.5370.1735. Combinatorial Electrochemistry: A Highly Parallel, Optical Screening Method for Discovery of Better Electrocatalysts

Combinatorial Electrochemistry: A Highly Parallel, Optical Screening Method for Discovery of Better Electrocatalysts

10.1126/science.280.5370.1735

Crossref journal-article

American Association for the Advancement of Science (AAAS)

Science (221)

Abstract

Combinatorial screening of electrochemical catalysts by current-voltage methods can be unwieldy for large sample sizes. By converting the ions generated in an electrochemical half-cell reaction to a fluorescence signal, the most active compositions in a large electrode array have been identified. A fluorescent acid-base indicator was used to image high concentrations of hydrogen ions, which were generated in the electrooxidation of methanol. A 645-member electrode array containing five elements (platinum, ruthenium, osmium, iridium, and rhodium), 80 binary, 280 ternary, and 280 quaternary combinations was screened to identify the most active regions of phase space. Subsequent “zoom” screens pinpointed several very active compositions, some in ternary and quaternary regions that were bounded by rather inactive binaries. The best catalyst, platinum(44)/ruthenium(41)/osmium(10)/iridium(5) (numbers in parentheses are atomic percent), was significantly more active than platinum(50)/ruthenium(50) in a direct methanol fuel cell operating at 60°C, even though the latter catalyst had about twice the surface area of the former.

Bibliography

Reddington, E., Sapienza, A., Gurau, B., Viswanathan, R., Sarangapani, S., Smotkin, E. S., & Mallouk, T. E. (1998). Combinatorial Electrochemistry: A Highly Parallel, Optical Screening Method for Discovery of Better Electrocatalysts. Science, 280(5370), 1735â1737.

Authors 7

Erik Reddington (first)
Anthony Sapienza (additional)
Bogdan Gurau (additional)
Rameshkrishnan Viswanathan (additional)
S. Sarangapani (additional)
Eugene S. Smotkin (additional)
Thomas E. Mallouk (additional)

References 31 Referenced 871

10.1126/science.1990438
Lam K. S., et al., Nature354, 82 (1991). (10.1038/354082a0) / Nature by Lam K. S. (1991)
R. A. Houghten et al. ibid. p. 84.
Bock L. C., Griffin L. C., Latham J. A., Vermann E. H., Toole J. J., ibid355, 564 (1992). / ibid by Bock L. C. (1992)
Cho C. Y., et al., Science261, 1303 (1993). (10.1126/science.7689747) / Science by Cho C. Y. (1993)
Bunin B. L., Ellman J. A., J. Am. Chem. Soc.114, 10997 (1992). (10.1021/ja00053a067) / J. Am. Chem. Soc. by Bunin B. L. (1992)
Virgilio A. A., Ellman J. A., ibid116, 11580 (1994). / ibid by Virgilio A. A. (1994)
DeWitt S. H., et al., Proc. Natl. Acad. Sci. U.S.A.90, 6909 (1993). (10.1073/pnas.90.15.6909) / Proc. Natl. Acad. Sci. U.S.A. by DeWitt S. H. (1993)
Campbell D. A., Bermak J. C., Burkoth T. S., Patel D. V., J. Am. Chem. Soc.117, 5381 (1995). (10.1021/ja00124a030) / J. Am. Chem. Soc. by Campbell D. A. (1995)
10.1073/pnas.90.23.10922
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J. J. Hanak J. Math. Sci. 5 964 (1970). (10.1007/BF00558177)
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van Dover R. B., Schneemeyer L. F., Fleming R. M., Nature392, 162 (1998). (10.1038/32381) / Nature by van Dover R. B. (1998)
Dickinson T. A., Walt D. R., White J., Kauer J. S., Anal. Chem.69, 3413 (1997). (10.1021/ac970501b) / Anal. Chem. by Dickinson T. A. (1997)
10.1126/science.270.5234.273
Xiang X.-D., et al., ibid268, 1738 (1995). / ibid by Xiang X.-D. (1995)
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McKee D. W., J. Catal.14, 355 (1969). (10.1016/0021-9517(69)90326-1) / J. Catal. by McKee D. W. (1969)
Metal salts were printed with an Apple Color Stylewriter 2500 onto Toray carbon rectangles taped to ordinary paper. The pattern for each element was drawn in gray scale with commercial drawing software. The printer was calibrated by ultraviolet-visible spectroscopy by printing a highly absorbing organic dye onto transparencies and then desorbing each spot into a known volume of solution. The reduction step was carried out by clamping the array into a home-built Plexiglas device that provided solution wells in the quaternary or five-pick-four pattern. In each well the printed metal salts were redissolved in a buffered solution (2 μl of 2 M NaHCO 3 ) and then reduced (1μl of 5% NaBH 4 ).
The aqueous indicator solution was 6 M methanol 0.5 M NaClO 4 30 mM Ni(ClO 4 ) 2 and 100 μM PTP adjusted to pH 3 with HClO 4 . The carbon substrate has a small resistance (1 to 3 ohms) which translates to a negligible potential drop at the screening currents used (about 1 mA). Bulk samples of catalysts were prepared by dissolving the appropriate metal salts in water to attain an overall concentration of 2 mM. The pH was adjusted to 9 and a 10-fold excess of 5 weight % sodium borohydride was added at one drop per minute. The black precipitate was washed 10 times with water and dried at 110°C. Fuel cell membrane-electrode assemblies were constructed from Nafion 117 by preparing a suspension of the catalyst in 15 weight % soluble Nafion and painting the material onto a decal as described in detail in (22).
We thank A. Czarnik D. L. Feldheim R. Wodd X.-D. Xiang and P. G. Schultz for helpful discussions; Todd LaFrenz for performing BET measurements; and the Office of Naval Research (LBL Molecular Design Institute) the Defense Advanced Research Projects Agency and the Army Research Office for financial support.

Dates

Type	When
Created	23 years ago (July 27, 2002, 5:43 a.m.)
Deposited	1 year, 7 months ago (Jan. 13, 2024, 12:27 a.m.)
Indexed	1 day, 5 hours ago (Aug. 21, 2025, 12:58 p.m.)
Issued	27 years, 2 months ago (June 12, 1998)
Published	27 years, 2 months ago (June 12, 1998)
Published Print	27 years, 2 months ago (June 12, 1998)

Funders 0

None

BibTeX

@article{Reddington_1998, title={Combinatorial Electrochemistry: A Highly Parallel, Optical Screening Method for Discovery of Better Electrocatalysts}, volume={280}, ISSN={1095-9203}, url={http://dx.doi.org/10.1126/science.280.5370.1735}, DOI={10.1126/science.280.5370.1735}, number={5370}, journal={Science}, publisher={American Association for the Advancement of Science (AAAS)}, author={Reddington, Erik and Sapienza, Anthony and Gurau, Bogdan and Viswanathan, Rameshkrishnan and Sarangapani, S. and Smotkin, Eugene S. and Mallouk, Thomas E.}, year={1998}, month=jun, pages={1735–1737} }

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