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Kernel Tuning and the Non-uniform Influence on Optical and Electrochemical Gaps of Bimetal Nanoclusters Lizhong He, Jinyun Yuan, Nan Xia, Lingwen Liao, Xu Liu, Zibao Gan, Chengming Wang, Jinlong Yang, and Zhikun Wu J. Am. Chem. Soc., Just Accepted Manuscript • DOI: 10.1021/jacs.7b12083 • Publication Date (Web): 22 Feb 2018 Downloaded from http://pubs.acs.org on February 22, 2018
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Kernel Tuning and the Non-uniform Influence on Optical and Electrochemical Gaps of Bimetal Nanoclusters Lizhong He+[a][b], Jinyun Yuan+ [c], Nan Xia[a], Lingwen Liao[a], Xu Liu[a][b], Zibao Gan[a], Chengming Wang[c], Jinlong Yang* [c], and Zhikun Wu*[a] [a]
Key Laboratory of Materials Physics, Anhui Key Laboratory of Nanomaterials and Nanotechnology, CAS Center for Excellence in Nanoscience, Institute of Solid State Physics, Chinese Academy of Sciences, Hefei 230031 (P. R. China) [b] University of Science and Technology of China, Hefei 230026 (P. R. China) [c] Hefei National Laboratory for Physical Sciences at the Microscale Institution, University of Science and Technology of China, Hefei 230026 (P. R. China) Supporting Information Placeholder ABSTRACT: Fine tuning nanoparticles with atomic precision is exciting and challenging and is critical for tuning the properties, understanding the structure-property correlation and determining the practical applications of nanoparticles. Some ultrasmall thiolated metal nanoparticles (metal nanoclusters) have been shown to be precisely doped, and even the protecting staple metal atom could be precisely reduced. However, the precise addition or reduction of the kernel atom while the other metal atoms in the nanocluster remain the same has not been successful until now to the best of our knowledge. Here, by carefully selecting the protecting ligand with adequate steric hindrance, we synthesized a novel nanocluster, in which the kernel can be regarded as that formed by the addition of two silver atoms to both ends of the Pt@Ag12 icosohedral kernel of the Ag24Pt(SR)18 (SR: thiolate) nanocluster, as revealed by single crystal X-ray crystallography. Interestingly, compared with the previously reported Ag24Pt(SR)18 nanocluster, the as-obtained novel bi-metal nanocluster exhibits a similar absorption but a different electrochemical gap. One possible explanation for this result is that the kernel tuning does not essentially change the electronic structure, but obviously influences the charge on the Pt@Ag12 kernel, as demonstrated by natural population analysis, thus possibly resulting in the large electrochemical gap difference between the two nanoclusters. This work not only provides a novel strategy to tune metal nanoclusters but also reveals that the kernel change does not necessarily alter the optical and electrochemical gaps in a uniform manner, which has important implications for the structure-property correlation of nanoparticles.
Metal nanoparticles have attracted great and enduring interest for years.1 Controlling the structure of metal nanoparticles with atomic precision is challenging1j, 1k, 2 yet critical for understanding the structure-property correlations,3 tuning the nanoparticle properties,4 and determining their practical applications.5 This goal was accomplished in ultrasmall thiolated metal nanoparticles (so-called metal nanoclusters) with the recent development of wet-chemistry approaches,1j, 1k, 6 thus greatly increasing the research on metal nanoclusters. It is generally believed that metal nanoclusters are composed of a pure metal kernel and ligand-containing staples,2a, 7 both of which can be precisely doped with a second metal.8 Recently, it was reported that the staple atoms could be precisely reduced via a two-step
anti-galvanic reduction process.4d, 6c, 9 However, precisely adding or removing the kernel atoms while the other metal atoms in the nanocluster remain the same (the protecting ligand can be changed) has not been reported so far to the best of our knowledge and is destined to be challenging since the kernel atoms are inside and are shielded by the outer staples. The kernel greatly influences the properties of nanoclusters3b, 3e, 4a, 8c, 10,11 (e.g., the electrochemical gap11); therefore, kernel tuning is not only interesting, useful and challenging but also very helpful for understanding the kernel-property correlation of metal nanoclusters. The electrochemical gap between the first oxidation and the first reduction potential (electrochemical gap for short) is correlated to the optical gap for metal nanoclusters;8f, 11c, 12 thus, a question that arises is whether the kernel tuning influences both of them to a comparable extent. These interesting and significant issues have stimulated the present research. Alloy nanoclusters were chosen as the synthesis target because alloy nanoclusters have more promosing properties than monometal nanoclusters because of synergy and counteraction effects.13 Among the various alloy nanoclusters, the H@M12@M12-type ones (H represents the hetero-metal atom, and M represents the metal atom) are ideal models4c,14 to study the doping effect and thus have received extensive interest recently. After many attempts, we successfully synthesized a novel nanocluster by carefully selecting the protecting ligand, which has a Pt@AgAg12Ag@Ag12 (or Pt@Ag14@Ag12) structure. Interestingly, compared with the previously reported Pt@Ag12@Ag12 structure,14d, 15 the novel alloy nanocluster exhibits a similar absorption (including the optical gap) but a different electrochemical gap. The intrinsic reason for this paradox is also discussed in this work, which will be detailed below. The sizes and structures of gold nanoclusters are sensitive to subtle changes in the surface protecting ligands; for example, Jin et al. synthesized three magic-sized nanoclusters (Au130(p-MBT)50, Au104(m-MBT)41 and Au40(o-MBT)24) by employing para-, metaand ortho-methyl benzenethiol, respectively.16 In a previous work, Ag24Pt(SR)18 (SR: thiolate) (Ag24Pt for short) was obtained using 2,4-dimethylbenzenethiol as the protecting ligand,14d, 15 and then, we conceived that a ligand with various steric hindrances in the ortho-position of phenthiol might lead to a nanocluster with a different kernel from that of Ag24Pt. Indeed, we succeeded in synthesizing such a nanocluster by employing 2-ethylbenzenethiol as the protecting ligand, indicating that the steric hindrance tuning at some position of the ligands is also an effective strategy to
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control the structure of metal nanoclusters. For the structure difference illustration between 2-ethylbenzenethiol and 2,4-dimethylbenzenethiol, see Figure S1. Note that other ligands, such as 3-ethylbenzenethiol,4-ethylbenzenethiol,4-tert-butylbenzenethiola te, 3, 4-difluorothiophenol, 3-bromothiophenol, 2-bromothiophenol and 2-methylbenzenethiol, are not adequate for the synthesis of a similar structure under similar conditions, implying that the increase in steric hindrance at the ortho-position of phenthiol may be critical for the synthesis of the target nanocluster (see supporting information for the details).
the icosahedral Pt@Ag12 of the Ag24Pt nanocluster and longer than the Ag-Ag bond lengths (average of 2.88 Å) in the icosahedral Pt@Ag12 of the biicosahedral Pt2Ag23Cl7(PPH3)10 nanocluster.8i The bipyramidal Pt@Ag14 kernel was protected by six dimeric (-SR-Ag-SR-Ag-PR3-) staple motifs, resembling the Pt@Ag12 kernel of Ag24Pt except that a -SR in the dimeric (-SR-Ag-SR-Ag-PR3-) staple motif of Ag24Pt was replaced by a -PR3, and six bridging µ3-S atoms were also present on the surface of the PtAg14 kernel. Note that the outer shell of Ag26Pt has the same number (12) of silver atoms as that of Ag24Pt, as shown in Figure 2. Thus the two nanoclusters have the same 8-electron superatomic structure but different charge state (0 vs -2). Despite the above-mentioned differences in composition and structure, the two nanoclusters have almost superimposable UV/vis/NIR spectra (including the optical gap), as shown in Figure 3a, indicating that they have highly similar electronic structures. The density function theory (DFT) calculation also reveals that the HOMO/LUMO are mainly localized at the PtAg12 kernel for both nanoclusters, as shown in Figure 4. The two “hub” silver atoms only slightly contribute to the HOMO/LUMO.
Figure 1. X-ray structure of the Ag26Pt nanocluster. (Color scheme: blue, platinum; red, silver; yellow, sulfur; pink, phosphorus; dark gray, carbon; white, hydrogen) The single crystal structure was resolved by X-ray crystallography. As shown in Figure 1, the nanocluster consists of 1 Pt atom, 26 silver atoms, 18 2-ethylbenzenethiolates and 6 PPH3. No counter-ion was found in the single crystal packing structure; thus, the nanocluster formula was determined to be Ag26Pt(2-EBT)18(PPh3)6 (2-EBTH = 2-ethylbenzenethiol, Ag26Pt for short), which was further supported by thermogravimetric analysis (TGA) as shown in Figure S2 and X-ray photoelectron spectroscopy (XPS). A weight loss of 57.2 wt % is in good agreement with the theoretical values of the Ag26Pt nanocluster (organic, 57.4 wt %; metal, 42.6 wt %). XPS analysis also shows that the Ag/Pt atomic ratio is 25.6/1(expected: 26/1). In addition, XPS confirms the existence of Ag, Pt, S, P, N and C and excludes other elements such as O and Cl, as shown in Figures S3 and S4. NMR provides another support for the structure and indicates that the ligand distribution on the Ag26Pt cluster crystal remains the same in solution form, see Figure S5 (for comparison, the NMR spectra of Ag24Pt are also provided, see Figure S6). The structural anatomy reveals that the metal atoms in the nanocluster have a concentric three-shell Pt@Ag14@Ag12 Keplerate packing, similar to that of Ag24Pt(2,4-DMBT)18 (Pt@Ag12@Ag12, 2,4-DMBTH = 2,4-dimethylbenzenethiol), except that the intershell can be regarded as the addition of two atoms to both ends of the icosohedral Pt@Ag12 of Ag24Pt, as illustrated in Figure 2b. From another perspective, the bimetal bipyramidal kernel can be viewed as an icosahedral PtAg12 connected with two Ag4 tetrahedra by sharing two Ag3 facets, as shown in Figure 2b, or it can be viewed as being constructed of 24 Ag3 facets (icositetrahedron). The Pt-Ag bond distances in the Pt@Ag12 icosahedral kernel of the Ag26Pt nanocluster range from 2.7514 Å to 2.7532 Å with an average of 2.7523 Å, which is slightly shorter than the Pt-Ag bond (2.7541 Å) in the Ag24Pt nanocluster. The Ag-Ag bond lengths in the icosahedral Pt@Ag12 of Ag26Pt average 2.9133 Å, which is slightly longer than the mean Ag-Ag bond length (2.9067 Å) in
Figure 2. Schematic illustration of the Ag26Pt and Ag24Pt nanocluster structures. (Color scheme: green, platinum; red, light green and blue, silver; yellow, sulfur; pink, phosphorus; all carbon and hydrogen atoms are omitted for clarity) Interestingly, regardless of the absorption identity, their differential pulse voltammetry (DPV) spectra show distinct differences, in particular, the electrochemical gap has a large margin (~0.41 V), see Figures 3b and 3c, which indicates that the kernel tuning does not necessarily alter both the optical and electrochemical gap. Such an inconsistence change between the electrochemical and optical gap of metal nanoclusters is not previously reported to the best of our knowledge. Note that, our case is also different from the case of neutral and anionic monometallic Au25 clusters, in which they show same electrochemistry but different absorption.17 The natural population analysis (NPA) gives a charge value of 0.06279 for the Pt@Ag12 unit in Ag26Pt but a value of -0.72028 for the Pt@Ag12 kernel in Ag24Pt, indicating that the negative charge in the Pt@Ag12 kernel of Ag24Pt is obviously greater than that in the Pt@Ag12 unit of Ag26Pt. The charge variation might account for the difference in the electrochemical gap since it influences the communication between the electrodes and nanoclusters. The fact that the electrochemical gap (1.60 V, see Figure S7) of Ag25(SR)18- with a charge value of -0.25083 falls in between the above mentioned two (1. 48 and 1.89 V, see Figure 3) provide a support for this speculation. Ag24Pt and Ag26Pt have various charges, however, they have very similar absorption, indicating that on the other hand the charge is not critical to the UV-vis absorption spectrum.
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In summary, we obtained a novel Ag-Pt bimetal nanocluster by carefully selecting the protecting ligand with adequate steric hindrance and resolved its structure by single-crystal X-ray crystallography (SCXC), which revealed that the as-obtained nanocluster consisted of a bipyramidal Pt@Ag14 kernel protected by six dimeric (-SR-Ag-SR-Ag-PR3-) staple motifs and six additional bridging µ3-S atoms. The Pt@Ag14 kernel can be regarded as that formed by the addition of two silver atoms to the icosohedral Pt@Ag12 kernel. From another perspective, the bipyramidal PtAg14 kernel is an icositetrahedron constructed by sharing two Ag3 facets between the icosahedral Pt@Ag12 and the two connected Ag4 tetrahedra. Regardless of the differences in composition and structure, both Ag26Pt and Ag24Pt are 8-electron superatoms and have highly similar electronic structures, which was illustrated by their almost superimposable UV/vis/NIR
spectra and the very similar HOMO/LUMO locations. However, these superatoms have very different electrochemical gaps, probably caused by the distinct differences in the charge of the Pt@Ag12 kernel, as indicated by the NPA. Thus, the change in the spatial structure in our case does not essentially influence the electronic structure but remarkably alters the charge on the Pt@Ag12 kernel of the Ag24Pt nanocluster. Thus, the kernel change does not necessarily alter the optical and electrochemical gaps in a uniform manner. Our work might introduce a new strategy for nanocluster tuning by changing the steric hindrance at some position of the protecting ligand, provide novel insights into the structure and properties of metal nanoclusters, and have important implications for the structure-property correlation of metal nanoclusters.
Figure 3. UV-visible absorption spectra of Ag26Pt and Ag24Pt nanoclusters (a), and differential pulse voltammetry (DPV) spectra of Ag26Pt (b) and Ag24Pt (c). (The redox wave at -1.1 V in Figure 3b is attributed to the residual O2 that was not completely removed by the degassing.12,18)
Figure 4. The electron densities of the HOMO, HOMO-1 HOMO-2 and LUMO, LUMO+1 of the Ag26Pt nanocluster (a-e) and the Ag24Pt nanocluster (f-j).
ASSOCIATED CONTENT
AUTHOR INFORMATION
Supporting Information
Corresponding Author
The Supporting Information is available free of charge on the ACS Publications website at http://pubs.acs.org. Experimental details and data (PDF). Crystallographic data for Ag26Pt(2-EBT)18(PPh3)6(CIF).
* E-mail:
[email protected],
[email protected] Author Contributions +
L. He and J. Yuan contributed equally to this work.
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Notes The authors declare no competing financial interests.
ACKNOWLEDGMENT The authors would like to thank Natural Science Foundation of China (Nos. 21171170, 21222301, 21771186, 21528303, 21603234, 21501182), and the CAS/SAFEA International Partnership Program for Creative Research Teams for financial support.
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