Amorphous-Phase-Mediated Crystallization of Ni Nanocrystals Revealed by High-Resolution Liquid-Phase Electron Microscopy.

Nonclassical features of crystallization in solution have been recently identified both experimentally and theoretically. In particular, an amorphous-phase-mediated pathway is found in various crystallization systems as an important route, different from the classical nucleation and growth model. Here, we utilize high-resolution in situ transmission electron microscopy with graphene liquid cells to study amorphous-phase-mediated formation of Ni nanocrystals. An amorphous phase is precipitated in the initial stage of the reaction. Within the amorphous particles, crystalline domains nucleate and eventually form nanocrystals. In addition, unique crystallization behaviors, such as formation of multiple domains and dislocation relaxation, are observed in amorphous-phase-mediated crystallization. Theoretical calculations confirm that surface interactions can induce amorphous precipitation of metal precursors, which is analogous to the surface-induced amorphous-to-crystalline transformation occurring in biomineralization. Our results imply that an unexplored nonclassical growth mechanism is important for the formation of nanocrystals.

[1]  T. Hyeon,et al.  Co2+-Doping of Magic-Sized CdSe Clusters: Structural Insights via Ligand Field Transitions. , 2018, Nano letters.

[2]  Kai He,et al.  In Situ Observation of Resistive Switching in an Asymmetric Graphene Oxide Bilayer Structure. , 2018, ACS nano.

[3]  N. de Jonge,et al.  Strategies for Preparing Graphene Liquid Cells for Transmission Electron Microscopy. , 2018, Nano letters.

[4]  N. Jonge Theory of the spatial resolution of (scanning) transmission electron microscopy in liquid water or ice layers , 2018 .

[5]  K. Yin,et al.  In-situ liquid cell transmission electron microscopy investigation on oriented attachment of gold nanoparticles , 2018, Nature Communications.

[6]  H. Pan,et al.  Amorphous Phase Mediated Crystallization: Fundamentals of Biomineralization , 2018 .

[7]  T. Hyeon,et al.  Liquid‐Phase Transmission Electron Microscopy for Studying Colloidal Inorganic Nanoparticles , 2018, Advanced materials.

[8]  N. de Jonge Theory of the spatial resolution of (scanning) transmission electron microscopy in liquid water or ice layers. , 2018, Ultramicroscopy.

[9]  Yeonwoong Jung,et al.  Tailoring crystallization phases in metallic glass nanorods via nucleus starvation , 2017, Nature Communications.

[10]  Won Chul Lee,et al.  Self-organized growth and self-assembly of nanostructures on 2D materials , 2017 .

[11]  S. Pennycook The impact of STEM aberration correction on materials science. , 2017, Ultramicroscopy.

[12]  Haimei Zheng,et al.  Visualization of Colloidal Nanocrystal Formation and Electrode-Electrolyte Interfaces in Liquids Using TEM. , 2017, Accounts of chemical research.

[13]  U. Mirsaidov,et al.  Direct Observation of Interactions between Nanoparticles and Nanoparticle Self-Assembly in Solution. , 2017, Accounts of chemical research.

[14]  Taeghwan Hyeon,et al.  Chemical Synthesis, Doping, and Transformation of Magic-Sized Semiconductor Alloy Nanoclusters. , 2017, Journal of the American Chemical Society.

[15]  Qian Chen,et al.  Quantifying the Self-Assembly Behavior of Anisotropic Nanoparticles Using Liquid-Phase Transmission Electron Microscopy. , 2017, Accounts of chemical research.

[16]  K. Tsukamoto,et al.  Two types of amorphous protein particles facilitate crystal nucleation , 2017, Proceedings of the National Academy of Sciences.

[17]  P. Král,et al.  Multistep nucleation of nanocrystals in aqueous solution. , 2016, Nature chemistry.

[18]  Qian Chen,et al.  In Situ Electron Microscopy Imaging and Quantitative Structural Modulation of Nanoparticle Superlattices. , 2016, ACS nano.

[19]  K. Jensen,et al.  Characterization of Indium Phosphide Quantum Dot Growth Intermediates Using MALDI-TOF Mass Spectrometry. , 2016, Journal of the American Chemical Society.

[20]  Ting Qi,et al.  General low-temperature reaction pathway from precursors to monomers before nucleation of compound semiconductor nanocrystals , 2016, Nature Communications.

[21]  N. Sommerdijk,et al.  Investigating materials formation with liquid-phase and cryogenic TEM , 2016 .

[22]  Taeghwan Hyeon,et al.  Nonclassical nucleation and growth of inorganic nanoparticles , 2016 .

[23]  L. Manna,et al.  In situ microscopy of the self-assembly of branched nanocrystals in solution , 2016, Nature Communications.

[24]  F. Ross Opportunities and challenges in liquid cell electron microscopy , 2015, Science.

[25]  Y. Chu,et al.  In Situ Study of Fe3Pt-Fe2O3 Core-Shell Nanoparticle Formation. , 2015, Journal of the American Chemical Society.

[26]  J. Banfield,et al.  Crystallization by particle attachment in synthetic, biogenic, and geologic environments , 2015, Science.

[27]  David T. Limmer,et al.  3D structure of individual nanocrystals in solution by electron microscopy , 2015, Science.

[28]  James E. Evans,et al.  Observing the growth of metal-organic frameworks by in situ liquid cell transmission electron microscopy. , 2015, Journal of the American Chemical Society.

[29]  Paul J. M. Smeets,et al.  Calcium carbonate nucleation driven by ion binding in a biomimetic matrix revealed by in situ electron microscopy. , 2015, Nature materials.

[30]  R. Klie,et al.  Heterogeneous nucleation and shape transformation of multicomponent metallic nanostructures. , 2015, Nature materials.

[31]  E. Sutter,et al.  Determination of redox reaction rates and orders by in situ liquid cell electron microscopy of Pd and Au solution growth. , 2014, Journal of the American Chemical Society.

[32]  S. Aloni,et al.  In situ TEM imaging of CaCO3 nucleation reveals coexistence of direct and indirect pathways , 2014, Science.

[33]  Lin-Wang Wang,et al.  Facet development during platinum nanocube growth , 2014, Science.

[34]  Lennart Bergström,et al.  Pre-nucleation clusters as solute precursors in crystallisation. , 2014, Chemical Society reviews.

[35]  M. Batzill,et al.  Graphene-nickel interfaces: a review. , 2014, Nanoscale.

[36]  R. Nuzzo,et al.  Noncrystalline-to-crystalline transformations in Pt nanoparticles. , 2013, Journal of the American Chemical Society.

[37]  A Paul Alivisatos,et al.  3D motion of DNA-Au nanoconjugates in graphene liquid cell electron microscopy. , 2013, Nano letters.

[38]  P. Fratzl,et al.  Nucleation and growth of magnetite from solution. , 2013, Nature materials.

[39]  C. Mirkin,et al.  Stepwise Evolution of Spherical Seeds into 20-Fold Twinned Icosahedra , 2012, Science.

[40]  S. Whitelam,et al.  Real-Time Imaging of Pt3Fe Nanorod Growth in Solution , 2012, Science.

[41]  Daniel J. Hellebusch,et al.  High-Resolution EM of Colloidal Nanocrystal Growth Using Graphene Liquid Cells , 2012, Science.

[42]  Niels de Jonge,et al.  Electron microscopy of specimens in liquid. , 2011, Nature nanotechnology.

[43]  P. C. Gibbons,et al.  Lamellar assembly of cadmium selenide nanoclusters into quantum belts. , 2011, Journal of the American Chemical Society.

[44]  A Paul Alivisatos,et al.  Precursor conversion kinetics and the nucleation of cadmium selenide nanocrystals. , 2010, Journal of the American Chemical Society.

[45]  F. Müller,et al.  The role of prenucleation clusters in surface-induced calcium phosphate crystallization. , 2010, Nature materials.

[46]  Andreas Kornowski,et al.  Ultrathin PbS Sheets by Two-Dimensional Oriented Attachment , 2010, Science.

[47]  V. Radmilović,et al.  Quantitative Li Mapping in Al alloys by Sub-eV Resolution Energy-Filtering Transmission Electron Microscopy (EFTEM) in the Aberration-Corrected, Monochromated TEAM0.5 Instrument , 2009, Microscopy and Microanalysis.

[48]  A. Alivisatos,et al.  Observation of Single Colloidal Platinum Nanocrystal Growth Trajectories , 2009, Science.

[49]  Helmut Cölfen,et al.  Stable Prenucleation Calcium Carbonate Clusters , 2008, Science.

[50]  Yang Li,et al.  Sequential Growth of Magic‐Size CdSe Nanocrystals , 2007 .

[51]  S. Vilminot,et al.  hcp and fcc Nickel Nanoparticles Prepared from Organically Functionalized Layered Phyllosilicates of Nickel(II) , 2007 .

[52]  A. Alivisatos,et al.  Mechanistic study of precursor evolution in colloidal group II-VI semiconductor nanocrystal synthesis. , 2007, Journal of the American Chemical Society.

[53]  S. Weiner,et al.  Sea Urchin Spine Calcite Forms via a Transient Amorphous Calcium Carbonate Phase , 2004, Science.

[54]  P. Mulvaney,et al.  Nucleation and growth kinetics of CdSe nanocrystals in octadecene , 2004 .

[55]  Xiaogang Peng,et al.  In Situ Observation of the Nucleation and Growth of CdSe Nanocrystals , 2004 .

[56]  F. Ross,et al.  Dynamic microscopy of nanoscale cluster growth at the solid–liquid interface , 2003, Nature materials.

[57]  Steve Weiner,et al.  Taking Advantage of Disorder: Amorphous Calcium Carbonate and Its Roles in Biomineralization , 2003 .

[58]  James J. De Yoreo,et al.  Principles of crystal nucleation and growth , 2003 .

[59]  A. Rogach,et al.  Evolution of an Ensemble of Nanoparticles in a Colloidal Solution: Theoretical Study , 2001 .

[60]  Ilhan A. Aksay,et al.  Biomimetic Synthesis of Macroscopic-Scale Calcium Carbonate Thin Films. Evidence for a Multistep Assembly Process , 1998 .

[61]  T. Sugimoto Preparation of monodispersed colloidal particles , 1987 .

[62]  N. Guglielmi Kinetics of the Deposition of Inert Particles from Electrolytic Baths , 1972 .