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Title: Solvent manipulation of the pre-reduction metal–ligand complex and particle-ligand binding for controlled synthesis of Pd nanoparticles

Abstract

Understanding how to control the nucleation and growth rates is crucial for designing nanoparticles with specific sizes and shapes. Herein, we show that the nucleation and growth rates are correlated with the thermodynamics of metal–ligand/solvent binding for the pre-reduction complex and the surface of the nanoparticle, respectively. To obtain these correlations, we measured the nucleation and growth rates by in situ small angle X-ray scattering during the synthesis of colloidal Pd nanoparticles in the presence of trioctylphosphine in solvents of varying coordinating ability. The results show that the nucleation rate decreased, while the growth rate increased in the following order, toluene, piperidine, 3,4-lutidine and pyridine, leading to a large increase in the final nanoparticle size (from 1.4 nm in toluene to 5.0 nm in pyridine). Using density functional theory (DFT), complemented by 31P nuclear magnetic resonance and X-ray absorption spectroscopy, we calculated the reduction Gibbs free energies of the solvent-dependent dominant pre-reduction complex and the solvent-nanoparticle binding energy. The results indicate that lower nucleation rates originate from solvent coordination which stabilizes the pre-reduction complex and increases its reduction free energy. At the same time, DFT calculations suggest that the solvent coordination affects the effective capping of the surface where strongermore » binding solvents slow the nanoparticle growth by lowering the number of active sites (not already bound by trioctylphosphine). The findings represent a promising advancement towards understanding the microscopic connection between the metal–ligand thermodynamic interactions and the kinetics of nucleation and growth to control the size of colloidal metal nanoparticles.« less

Authors:
 [1];  [2];  [2];  [1]; ORCiD logo [2]; ORCiD logo [3];  [4]; ORCiD logo [5];  [1]; ORCiD logo [1]; ORCiD logo [6]; ORCiD logo [2]; ORCiD logo [1]
+ Show Author Affiliations
  1. Virginia Polytechnic Inst. and State Univ. (Virginia Tech), Blacksburg, VA (United States)
  2. Univ. of Pittsburgh, PA (United States)
  3. Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
  4. Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
  5. Argonne National Lab. (ANL), Argonne, IL (United States)
  6. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Publication Date:
Research Org.:
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL); Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Pacific Northwest National Laboratory (PNNL), Richland, WA (United States). Environmental Molecular Sciences Laboratory (EMSL); Los Alamos National Laboratory (LANL), Los Alamos, NM (United States). Center for Integrated Nanotechnologies (CINT)
Sponsoring Org.:
National Science Foundation (NSF); USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Science (SC), Biological and Environmental Research (BER); USDOE National Nuclear Security Administration (NNSA)
OSTI Identifier:
1763295
Alternate Identifier(s):
OSTI ID: 1756217; OSTI ID: 1818454; OSTI ID: 1856172
Report Number(s):
PNNL-SA-158241; LA-UR-21-30400
Journal ID: ISSN 2040-3364
Grant/Contract Number:  
AC05-76RL01830; CHE-1507370; AC02-76SF00515; SC0012335; AC02-06CH11357; AC52-06NA25396; 1652694; 1247842; 89233218CNA000001
Resource Type:
Accepted Manuscript
Journal Name:
Nanoscale
Additional Journal Information:
Journal Volume: 13; Journal Issue: 1; Journal ID: ISSN 2040-3364
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Inorganic and Physical Chemistry; Material Science

Citation Formats

Li, Wenhui, Taylor, Michael G., Bayerl, Dylan, Mozaffari, Saeed, Dixit, Mudit, Ivanov, Sergei A., Seifert, Soenke, Lee, Byeongdu, Shanaiah, Narasimhamurthy, Lu, Yubing, Kovarik, Libor, Mpourmpakis, Giannis, and Karim, Ayman M. Solvent manipulation of the pre-reduction metal–ligand complex and particle-ligand binding for controlled synthesis of Pd nanoparticles. United States: N. p., 2020. Web. doi:10.1039/d0nr06078j.
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Li, Wenhui, Taylor, Michael G., Bayerl, Dylan, Mozaffari, Saeed, Dixit, Mudit, Ivanov, Sergei A., Seifert, Soenke, Lee, Byeongdu, Shanaiah, Narasimhamurthy, Lu, Yubing, Kovarik, Libor, Mpourmpakis, Giannis, & Karim, Ayman M. Solvent manipulation of the pre-reduction metal–ligand complex and particle-ligand binding for controlled synthesis of Pd nanoparticles. United States. https://doi.org/10.1039/d0nr06078j
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Li, Wenhui, Taylor, Michael G., Bayerl, Dylan, Mozaffari, Saeed, Dixit, Mudit, Ivanov, Sergei A., Seifert, Soenke, Lee, Byeongdu, Shanaiah, Narasimhamurthy, Lu, Yubing, Kovarik, Libor, Mpourmpakis, Giannis, and Karim, Ayman M. Mon . "Solvent manipulation of the pre-reduction metal–ligand complex and particle-ligand binding for controlled synthesis of Pd nanoparticles". United States. https://doi.org/10.1039/d0nr06078j. https://www.osti.gov/servlets/purl/1763295.
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@article{osti_1763295,
title = {Solvent manipulation of the pre-reduction metal–ligand complex and particle-ligand binding for controlled synthesis of Pd nanoparticles},
author = {Li, Wenhui and Taylor, Michael G. and Bayerl, Dylan and Mozaffari, Saeed and Dixit, Mudit and Ivanov, Sergei A. and Seifert, Soenke and Lee, Byeongdu and Shanaiah, Narasimhamurthy and Lu, Yubing and Kovarik, Libor and Mpourmpakis, Giannis and Karim, Ayman M.},
abstractNote = {Understanding how to control the nucleation and growth rates is crucial for designing nanoparticles with specific sizes and shapes. Herein, we show that the nucleation and growth rates are correlated with the thermodynamics of metal–ligand/solvent binding for the pre-reduction complex and the surface of the nanoparticle, respectively. To obtain these correlations, we measured the nucleation and growth rates by in situ small angle X-ray scattering during the synthesis of colloidal Pd nanoparticles in the presence of trioctylphosphine in solvents of varying coordinating ability. The results show that the nucleation rate decreased, while the growth rate increased in the following order, toluene, piperidine, 3,4-lutidine and pyridine, leading to a large increase in the final nanoparticle size (from 1.4 nm in toluene to 5.0 nm in pyridine). Using density functional theory (DFT), complemented by 31P nuclear magnetic resonance and X-ray absorption spectroscopy, we calculated the reduction Gibbs free energies of the solvent-dependent dominant pre-reduction complex and the solvent-nanoparticle binding energy. The results indicate that lower nucleation rates originate from solvent coordination which stabilizes the pre-reduction complex and increases its reduction free energy. At the same time, DFT calculations suggest that the solvent coordination affects the effective capping of the surface where stronger binding solvents slow the nanoparticle growth by lowering the number of active sites (not already bound by trioctylphosphine). The findings represent a promising advancement towards understanding the microscopic connection between the metal–ligand thermodynamic interactions and the kinetics of nucleation and growth to control the size of colloidal metal nanoparticles.},
doi = {10.1039/d0nr06078j},
journal = {Nanoscale},
number = 1,
volume = 13,
place = {United States},
year = {Mon Nov 30 00:00:00 EST 2020},
month = {Mon Nov 30 00:00:00 EST 2020}
}
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  • Kwon, Soon Gu; Krylova, Galyna; Phillips, Patrick J.
  • Nature Materials, Vol. 14, Issue 2
  • DOI: 10.1038/nmat4115

Metal complexes of sulphur ligands. Part 17. Reaction of palladium(II) and platinum(II) monothiobenzoates with various Lewis bases and further studies on complexes containing related ligands
journal, January 1978

  • Goodfellow, John A.; Stephenson, T. Anthony; Cornock, Margaret C.
  • Journal of the Chemical Society, Dalton Transactions, Issue 9
  • DOI: 10.1039/DT9780001195

RI-MP2: first derivatives and global consistency
journal, October 1997

  • Weigend, Florian; Häser, Marco
  • Theoretical Chemistry Accounts: Theory, Computation, and Modeling (Theoretica Chimica Acta), Vol. 97, Issue 1-4
  • DOI: 10.1007/s002140050269

Ultra-large-scale syntheses of monodisperse nanocrystals
journal, November 2004

  • Park, Jongnam; An, Kwangjin; Hwang, Yosun
  • Nature Materials, Vol. 3, Issue 12
  • DOI: 10.1038/nmat1251
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