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@ARTICLE{Leffler:891844,
      author       = {Leffler, Vanessa and Ehlert, Sascha and Förster, Beate and
                      Dulle, Martin and Förster, Stephan},
      title        = {{N}anoparticle {H}eat-{U}p {S}ynthesis: {I}n {S}itu {X}-ray
                      {D}iffraction and {E}xtension from {C}lassical to
                      {N}onclassical {N}ucleation and {G}rowth {T}heory},
      journal      = {ACS nano},
      volume       = {15},
      number       = {1},
      issn         = {1936-086X},
      address      = {Washington, DC},
      publisher    = {Soc.},
      reportid     = {FZJ-2021-01767},
      pages        = {840 - 856},
      year         = {2021},
      abstract     = {Heat-up synthesis routes are very commonly used for the
                      controlled large-scale production of semiconductor and
                      magnetic nanoparticles with narrow size distribution and
                      high crystallinity. To obtain fundamental insights into the
                      nucleation and growth kinetics is particularly demanding,
                      because these procedures involve heating to temperatures
                      above 300 °C. We designed a sample environment to perform
                      in situ SAXS/WAXS experiments to investigate the nucleation
                      and growth kinetics of iron oxide nanoparticles during
                      heat-up synthesis up to 320 °C. The analysis of the growth
                      curves for varying heating rates, Fe/ligand ratios, and
                      plateau temperatures shows that the kinetics proceeds via a
                      characteristic sequence of three phases: an induction Phase
                      I, a final growth Phase III, and an intermediate Phase II,
                      which can be divided into an early phase with the evolution
                      and subsequent dissolution of an amorphous transient state,
                      and a late phase, where crystalline particle nucleation and
                      aggregation occurs. We extended classical nucleation and
                      growth theory to account for an amorphous transient state
                      and particle aggregation during the nucleation and growth
                      phases. We find that this nonclassical theory is able to
                      quantitatively describe all measured growth curves. The
                      model provides fundamental insights into the underlying
                      kinetic processes especially in the complex Phase II with
                      the occurrence of a transient amorphous state, the
                      nucleation of crystalline primary particles, particle
                      growth, and particle aggregation proceeding on overlapping
                      time scales. The described in situ experiments together with
                      the extension of the classical nucleation and growth model
                      highlight the two most important features of nonclassical
                      nucleation and growth routes, i.e., the formation of
                      intermediate or transient species and particle aggregation
                      processes. They thus allow us to quantitatively understand,
                      predict, and control nanoparticle nucleation and growth
                      kinetics for a wide range of nanoparticle systems and
                      synthetic procedures.},
      cin          = {ER-C-1},
      ddc          = {540},
      cid          = {I:(DE-Juel1)ER-C-1-20170209},
      pnm          = {535 - Materials Information Discovery (POF4-535)},
      pid          = {G:(DE-HGF)POF4-535},
      typ          = {PUB:(DE-HGF)16},
      pubmed       = {33393769},
      UT           = {WOS:000613942700061},
      doi          = {10.1021/acsnano.0c07359},
      url          = {https://juser.fz-juelich.de/record/891844},
}