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Crystal-Phase and Surface-Structure Engineering of Ruthenium Nanocrystals

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Crystal-Phase and Surface-Structure Engineering of Ruthenium Nanocrystals REVIEWS Crystal-phase and surface-structure engineering of ruthenium nanocrystals Ming Zhao 1 and Younan Xia 1,2,3 ✉ Abstract | Metal nanocrystals with controlled shapes or surface structures have received increasing attention, owing to their desirable properties for applications ranging from catalysis to photonics, energy and biomedicine. Most studies, however, have been limited to nanocrystals with the same crystal phase as the bulk material. Engineering the phase of metal nanocrystals while simultaneously attaining shape-controlled synthesis has recently emerged as a new frontier of research. Here, we use Ru as an example to evaluate recent progress in the synthesis of metal nanocrystals featuring different crystal phases and well-controlled shapes. We first discuss synthetic strategies for controlling the crystal phase and shape of Ru nanocrystals, with a focus on new mechanistic insights. We then highlight the major factors that affect the packing of Ru atoms and, thus, the crystal phase, followed by an examination of the thermal stability of Ru nanocrystals in terms of both crystal phase and shape. Next, we showcase the successful implementation of these Ru nanocrystals in various catalytic applications. Finally , we end with a discussion of the challenges and opportunities in the field, including leveraging the lessons learned from Ru to engineer the crystal phase and surface structure of other metals. The past two decades have witnessed the development of metal nanocrystals7–11. Unlike shape control, which of new colloidal metal nanocrystals that are finding only involves surface atoms or a small portion of inter- widespread use in applications such as catalysis, energy nal atoms (such as twin boundaries and stacking faults), conversion and storage, photonics, electronics and bio- any modulation of the crystal structure requires the medicine1–5. However, in the case of noble metals, their rearrangement of all atoms to form a new lattice. As extreme scarcity in the Earth’s crust (typically at levels of such, the physical and chemical attributes of the result- parts per billion) and ever-increasing price have quickly ant nanocrystals can be substantially altered to enhance created a barrier to their large-scale use. To enable the their properties and performance. For example, when widespread use of noble metals in catalytic applications, Ru is crystallized in a body-centred cubic (bcc) structure, it is necessary to substantially reduce the amount of computational simulations show that the metal becomes metal needed by improving the catalytic performance. ferromagnetic, whereas bulk Ru in the hexagonal One effective strategy relies on shape-controlled synthe- close-packed (hcp) phase is paramagnetic12. sis, which enables the engineering of facets and, thus, of For a bulk solid material, the total energy is domi- 1School of Chemistry and the surface structure of nanocrystals1–5. For instance, a nated by the bulk energy, which is extremely difficult Biochemistry, Georgia systematic study of the facet-dependent activity of Pd to overcome to rearrange the atoms. When moving to Institute of Technology, nanocrystals towards formic-acid oxidation indicated nanocrystals, the surface energy plays a more impor- Atlanta, GA, USA. that the well-defined {100} facets of Pd nanocubes were tant role, making it feasible to attain nanocrystals with 2The Wallace H. Coulter Department of Biomedical 3.4 times more active than the poorly defined surface atomic packing different from that of the bulk mate- 6 13 Engineering, Georgia Institute of a commercial Pd/C catalyst . When {100} facets rial . For example, it was demonstrated that Pd nano- of Technology and Emory were combined with twin boundaries in Pd bipyrami- cubes can undergo a phase transition from face-centred University, Atlanta, GA, USA. dal nanocrystals, the specific activity showed a 5.2-fold cubic (fcc) to face-centred tetragonal (fct) at pressures 3School of Chemical and 6 (REF.14) enhancement relative to the commercial Pd/C catalyst . above 24.8 GPa . It was also reported that fcc-Pt3Co Biomolecular Engineering, Shape-controlled synthesis has been accomplished for nanocrystals with a random distribution of the Pt and Georgia Institute of Technology, Atlanta, GA, USA. almost all noble metals, with notable examples including Co atoms could be converted into Pt3−xCo@Ptx core– (REFS1–6) ✉e-mail: younan.xia@ Ag, Au, Pd, Pt and Rh . shell nanocrystals after annealing at 700 °C under H2 bme.gatech.edu In addition to shape control, people also search for atmosphere for 2 h. The Pt and Co atoms in the core https://doi.org/10.1038/ new control knobs, such as the crystal phase or struc- took a simple cubic packing for the generation of a s41578-020-0183-3 ture, that can be used to further enhance the properties L12 structure, and the core–shell nanocrystals showed 440 | JUNE 2020 | VOLUME 5 www.nature.com/natrevmats REVIEWS Pd@fcc-Ru core–shell icosahedra and Pd@fcc-Ru core–shell nanocubes and fcc-Ru fcc-Ru icosahedral nanocages covered cubic nanocages enclosed by {100} facets21 by {111} facets and twin boundaries23 Pd@fcc-Ru core–frame cuboctahedra and fcc-Ru nanoframes with Discovery of fcc Pd@fcc-Ru core–frame octahedra and fcc-Ru 4H/fcc Au@Ru core–branch nanowires a cuboctahedral shape50 structure in Ru nanoframes with an octahedral shape25 and 4H/fcc-Ru nanotubes46, 48 nanocrystals24 Rh@fcc-Ru core–shell Pd@fcc-Ru core–shell octahedra octahedra covered by Synthesis of pure fcc-Ru and fcc-Ru octahedral nanocages {111} facets and a shell nanocrystals with tunable sizes17 enclosed by {111} facets22 thickness of 4.5 nm (REF.39) 2010 2012 2013 2016 2017 2018 2019 hcp-Ru nanoplates with a hcp-Ru nanocrystals with hcp-Ru Au@Ru fcc-core–hcp-branch hcp-Ru nanobranches 32 triangular shape29 an hourglass shape30 nanochains25, 26 nanocrystals53 hcp-Ru nanocrystals with hcp-Ru nanowires Pd@Ru fcc-core–hcp-branch a capped-column with a polycrystalline nanocrystals54 morphology29 structure 28 Fig. 1 | Timeline showing key accomplishments in engineering the crystal and surface structures of Ru nanocrystals. 4H, hexagonal Bravais with four minimal repeating atomic layers (ABCB); fcc, face-centred cubic; hcp, hexagonal close-packed. substantial enhancements in both activity and durability (where H represents the hexagonal Bravais lattice and towards the oxygen-reduction reaction15. In addition to 4 stands for the number of minimal repeating atomic lay- the application of external stimuli (such as high pressure ers, ABCB), and that the deposited metals all possess the and/or high temperature), wet-chemical synthesis under same 4H phase20. Seed-mediated growth has also been ambient pressure and at relatively low temperature has applied to the facile synthesis of Ru nanocrystals with an also been explored to induce phase transitions in nano- fcc lattice and controlled surface structures, including the crystals. Under the right conditions, new crystal phases type of facet and the presence of twin boundaries21–23. can be produced and preserved during the homogene- Using Ru as an example, in this Review, we discuss ous nucleation process. Using this strategy, nanocrys- the recent progress in developing noble-metal nano- tals featuring new crystal phases have been achieved crystals with both new crystal structures and controlled for a number of noble metals, including hcp-Rh and shapes (Fig. 1). We choose to focus on Ru because it is fcc-Ru (REFS16,17). one of the very few metals that have been prepared as Despite the variation in crystal phase, the prod- nanocrystals purely in the hcp or fcc phase7,8,17. Metals ucts reported in those studies typically showed poorly are well known for their limited polymorphism and, defined shapes or morphologies, so that the bene- essentially, all of them crystallize in one of the three fits expected from shape control tended to vanish. crystal structures stable under atmospheric pressure: bcc, Regarding shape-controlled synthesis, essentially all hcp and fcc. All noble metals form the fcc phase except studies reported so far only dealt with noble metals that Ru and Os, which favour hcp. Ru can also exist in the fcc take an fcc structure1–6. In recent years, it was reported phase under atmospheric pressure when prepared as that small domains featuring hcp or other metastable nanoparticles17,24. Unlike for other noble metals such phases could emerge in fcc noble-metal nanocrystals as Ag, Au, Pd and Pt, there are only a limited number of as a consequence of stacking faults4,6. However, the publications on the synthesis of Ru nanocrystals. Most percentage of the new phase in the whole sample is of the products obtained through homogeneous nuclea- very small, typically below 5%. This predicament has tion are poorly defined in shape and of very small sizes, motivated people to develop new approaches to simul- typically below 5 nm (REFS24–27). There are only a few taneously control the crystal phase and shape of nano- reports on the homogeneous nucleation and growth crystals. In one method, one-pot synthesis was replaced of hcp-Ru nanocrystals in the shape of plates, discs, by seed-mediated growth, in which preformed seeds prisms or pyramids28–32. This can be attributed to the are introduced to direct the nucleation and growth of unique properties of Ru: the Ru3+/Ru pair has a much a metal of interest18,19. Relative to homogeneous nuclea- lower reduction potential than other noble metals, tion, heterogeneous nucleation has a lower energy bar- which makes it relatively difficult to produce Ru atoms rier and it allows one to finely manoeuvre the growth from a precursor through chemical reduction33; and Ru pattern. In particular, when nanocrystals with the thermodynamically favours the hcp structure, which, desired crystal phase and shape are leveraged as seeds, together with the very high cohesive and surface ener- one can simultaneously replicate both their crystal gies of Ru relative to those of other noble metals, makes phase and surface structure in the deposited metal18,19.
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