Facile synthesis of precious-metal single-site catalysts using organic solvents


Single-site catalysts can demonstrate high activity and selectivity in many catalytic reactions. The synthesis of these materials by impregnation from strongly oxidizing aqueous solutions or pH-controlled deposition often leads to low metal loadings or a range of metal species. Here, we demonstrate that simple impregnation of the metal precursors onto activated carbon from a low-boiling-point, low-polarity solvent, such as acetone, results in catalysts with an atomic dispersion of cationic metal species. We show the generality of this method by producing single-site Au, Pd, Ru and Pt catalysts supported on carbon in a facile manner. Single-site Au/C catalysts have previously been validated commercially to produce vinyl chloride, and here we show that this facile synthesis method can produce effective catalysts for acetylene hydrochlorination in the absence of the highly oxidizing acidic solvents previously used.

Access options

Rent or Buy article

Get time limited or full article access on ReadCube.


All prices are NET prices.

Fig. 1: Characterization of Ru/C, Pd/C, Pt/C and Au/C catalysts prepared by impregnation of metal precursors from acetone.
Fig. 2: Characterization and testing of a series of Au/C catalysts prepared by impregnation of the metal precursor from different solvents.
Fig. 3: Au L3-edge XAS characterization of the Au/C-acetone catalyst.
Fig. 4: Catalytic performance of the Au/C-acetone catalyst.
Fig. 5: Characterization and testing of Ru/C, Pd/C, Pt/C and Au/C catalysts prepared by impregnation of metal precursors from acetone.

Data availability

Data supporting the results presented here, including how to access them, can be found in the Cardiff University data catalogue at https://doi.org/10.17035/d.2020.0098831512.


  1. 1.

    Yang, X. F. et al. Single-atom catalysts: a new frontier in heterogeneous catalysis. Acc. Chem. Res. 46, 1740–1748 (2013).

    CAS  Article  Google Scholar 

  2. 2.

    Wei, H. et al. FeOx-supported platinum single-atom and pseudo-single-atom catalysts for chemoselective hydrogenation of functionalized nitroarenes. Nat. Commun. 5, 1–8 (2014).

    CAS  Google Scholar 

  3. 3.

    Vilé, G. et al. A stable single-site palladium catalyst for hydrogenations. Angew. Chem. Int. Ed. 54, 11265–11269 (2015).

    Article  Google Scholar 

  4. 4.

    Pei, G. X. et al. Ag alloyed Pd single-atom catalysts for efficient selective hydrogenation of acetylene to ethylene in excess ethylene. ACS Catal. 5, 3717–3725 (2015).

    CAS  Article  Google Scholar 

  5. 5.

    Chen, Z. et al. A heterogeneous single-atom palladium catalyst surpassing homogeneous systems for Suzuki coupling. Nat. Nanotechnol. 13, 1–6 (2018).

    Google Scholar 

  6. 6.

    Yang, S., Tak, Y. J., Kim, J., Soon, A. & Lee, H. Support effects in single-atom platinum catalysts for electrochemical oxygen reduction. ACS Catal. 7, 1301–1307 (2017).

    CAS  Article  Google Scholar 

  7. 7.

    Zhu, C., Shi, Q., Feng, S., Du, D. & Lin, Y. Single-atom catalysts for electrochemical water splitting. ACS Energy Lett. 3, 1713–1721 (2018).

    CAS  Article  Google Scholar 

  8. 8.

    He, Q. et al. Population and hierarchy of active species in gold iron oxide catalysts for carbon monoxide oxidation. Nat. Commun. 7, 1–8 (2016).

    Google Scholar 

  9. 9.

    Fu, Q. Active non-metallic Au and Pt species on ceria-based water–gas shift catalysts. Science 301, 935–938 (2003).

    CAS  Article  Google Scholar 

  10. 10.

    Li, X. et al. Graphitic carbon nitride supported single-atom catalysts for efficient oxygen evolution reaction. Chem. Commun. 52, 13233–13236 (2016).

    CAS  Article  Google Scholar 

  11. 11.

    Duan, H. et al. Single-site palladium(ii) catalyst for oxidative Heck reaction: catalytic performance and kinetic investigations. ACS Catal. 5, 3752–3759 (2015).

    CAS  Article  Google Scholar 

  12. 12.

    Malta, G. et al. Identification of single-site gold catalysis in acetylene hydrochlorination. Science 355, 1399–1403 (2017).

    CAS  Article  Google Scholar 

  13. 13.

    Johnston, P., Carthey, N. & Hutchings, G. J. Discovery, development, and commercialization of gold catalysts for acetylene hydrochlorination. J. Am. Chem. Soc. 137, 14548–14557 (2015).

    CAS  Article  Google Scholar 

  14. 14.

    Hutchings, G. J. Vapor phase hydrochlorination of acetylene: correlation of catalytic activity of supported metal chloride catalysts. J. Catal. 96, 292–295 (1985).

    CAS  Article  Google Scholar 

  15. 15.

    Liu, X. et al. Investigation of the active species in the carbon-supported gold catalyst for acetylene hydrochlorination. Catal. Sci. Technol. 6, 5144–5153 (2016).

    CAS  Article  Google Scholar 

  16. 16.

    Deng, W., De Jesus, J., Saltsburg, H. & Flytzani-Stephanopoulos, M. Low-content gold-ceria catalysts for the water–gas shift and preferential CO oxidation reactions. Appl. Catal. A 291, 126–135 (2005).

    CAS  Article  Google Scholar 

  17. 17.

    Qiao, B. et al. Single-atom catalysis of CO oxidation using Pt1/FeOx. Nat. Chem. 3, 634–641 (2011).

    CAS  Article  Google Scholar 

  18. 18.

    Lin, J. et al. Remarkable performance of Ir1/FeOx single-atom catalyst in water gas shift reaction. J. Am. Chem. Soc. 135, 15314–15317 (2013).

    CAS  Article  Google Scholar 

  19. 19.

    Pieker, W. A. An EXAFS study of the coordination chemistry of hydrogen hexachloroplatinate (iv): 2. Speciation of complexes adsorbed onto alumina. Appl. Catal. A 243, 53–66 (2003).

    Article  Google Scholar 

  20. 20.

    Miller, J. T., Schreiber, M., Kropf, J. & Regalbuto, J. R. A fundamental study of platinum tetraammine impregnation of silica: 2. The effect of method of preparation, loading, and calcination temperature on (reduced) particle size. J. Catal. 225, 203–212 (2004).

    CAS  Article  Google Scholar 

  21. 21.

    Malta, G., Freakley, S. J., Kondrat, S. A. & Hutchings, G. J. Acetylene hydrochlorination using Au/carbon: a journey towards single site catalysis. Chem. Commun. 53, 11733–11746 (2017).

    CAS  Article  Google Scholar 

  22. 22.

    Chang, S. Y. et al. Structure and bonding in Au(i) chloride species: a critical examination of X-ray absorption spectroscopy (XAS) data. RSC Adv. 5, 6912–6918 (2015).

    CAS  Article  Google Scholar 

  23. 23.

    Pantelouris, A., Küper, G., Hormes, J., Feldmann, C. & Jansen, M. Anionic gold in Cs3AuO and Rb3AuO established by X-ray absorption spectroscopy. J. Am. Chem. Soc. 117, 11749–11753 (1995).

    CAS  Article  Google Scholar 

  24. 24.

    Richardson, M. J., Johnston, J. H. & Borrmann, T. Monomeric and polymeric amines as dual reductants/stabilisers for the synthesis of gold nanocrystals: a mechanistic study. Eur. J. Inorg. Chem. 2006, 2618–2623 (2006).

    Article  Google Scholar 

  25. 25.

    Reichardt, C. Empirical parameters of solvent polarity as linear free-energy relationships. Angew. Chem Int. Ed. 18, 98–110 (1979).

    Article  Google Scholar 

  26. 26.

    Malta, G. et al. Deactivation of a single-site gold-on-carbon acetylene hydrochlorination catalyst: an X-ray absorption and inelastic neutron scattering study. ACS Catal. 8, 8493–8505 (2018).

    CAS  Article  Google Scholar 

  27. 27.

    O’Connell, K. C., Monnier, J. R. & Regalbuto, J. R. The curious relationship of sintering to activity in supported gold catalysts for the hydrochlorination of acetylene. Appl. Catal. B 225, 264–272 (2018).

    Article  Google Scholar 

  28. 28.

    Ravel, B. & Newville, M. ATHENA, ARTEMIS, HEPHAESTUS: data analysis for X-ray absorption spectroscopy using IFEFFIT. J. Synchrotron Rad. 12, 537–541 (2005).

    CAS  Article  Google Scholar 

Download references


The authors thank Cardiff University for financial support. X.S. thanks the China Scholarship Council (CSC) for his scholarship. S.J.F. acknowledges the Ser Cymru II Fellowship scheme part-funded by the European Regional Development Fund. C.J.K. acknowledges funding from the National Science Foundation Major Research Instrumentation program (GR MRI/DMR-1040229). We thank Diamond Light Source for access and support in the use of the Electron Physical Science Imaging Centre (ePSIC Instrument E01 with proposal numbers MG22766-1 and EM20643-2 (with R. Wang, University College London)). We acknowledge Diamond Light Source for time on Beamline B18 under proposals SP19580-1, SP19850-2 and SP19580-3.

Author information




Catalysts were prepared, tested and characterized by X.S., S.R.D., T.E.P. and G.M. under the supervision of S.A.K., S.J.F. and G.J.H. Microscopy was carried out by T.E.D., Q.H. and L.L. under the supervision of C.J.K. XPS was carried out by D.J.M and T.E.P., and testing under industrial conditions was carried out by N.C. and P.J. The manuscript was written by S.J.F., S.A.K., G.M. and G.J.H. with input from all authors.

Corresponding author

Correspondence to Graham J. Hutchings.

Ethics declarations

Competing interests

The authors declare no competing interests.

Additional information

Publisher’s note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Supplementary information

Supplementary Information

Supplementary Tables 1–6 and Figs. 1–16.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Sun, X., Dawson, S.R., Parmentier, T.E. et al. Facile synthesis of precious-metal single-site catalysts using organic solvents. Nat. Chem. 12, 560–567 (2020). https://doi.org/10.1038/s41557-020-0446-z

Download citation

Further reading


Nature Briefing

Sign up for the Nature Briefing newsletter — what matters in science, free to your inbox daily.

Get the most important science stories of the day, free in your inbox. Sign up for Nature Briefing