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  3. Autonomous Nanoparticle Synthesis Guided By In Situ Multiscale Structural Characterization.
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  3. Autonomous Nanoparticle Synthesis Guided By In Situ Multiscale Structural Characterization.

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Autonomous Nanoparticle Synthesis Guided by In Situ Multiscale Structural Characterization.

Hyeong Jin Kim1, Matthew R Carbone2, Fang Lu1

  • 1Center for Functional Nanomaterials, Brookhaven National Laboratory, Upton, New York 11973, United States.

Journal of the American Chemical Society
|December 24, 2025

View abstract on PubMed

Summary
This summary is machine-generated.

This study presents an autonomous platform for nanoparticle synthesis, enabling precise control over gold nanoparticle size and structure. The system efficiently optimizes synthesis parameters, advancing automated materials discovery.

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Area of Science:

  • Materials Science
  • Nanotechnology
  • Chemical Engineering

Background:

  • Autonomous synthesis platforms offer rapid exploration of chemical parameter spaces.
  • Integrating in situ structural characterization with closed-loop synthesis optimization is a significant challenge.

Purpose of the Study:

  • To develop and demonstrate a closed-loop autonomous platform for synthesizing gold nanoparticles with targeted characteristics.
  • To achieve precise control over nanoparticle size and polydispersity using in situ structural characterization.

Main Methods:

  • Coupling a droplet-flow microreactor with in situ X-ray scattering (SAXS/WAXS) and Gaussian process optimization.
  • Exploring a vast parameter space (∼19,000 recipes) through automated experimentation.
  • Utilizing quantitative SAXS/WAXS and electron microscopy for structural analysis.

Main Results:

  • Achieved precise control over gold nanoparticle size (4-60 nm) and low polydispersity (σ < 0.11).
  • Discovered a universal relationship between crystallite size and particle size (dc = 0.18d + β), with synthesis chemistry controlling the intercept.
  • Demonstrated independent tuning of crystallite domain size at fixed particle diameter.

Conclusions:

  • The developed closed-loop platform provides a robust framework for mapping and controlling multiscale nanoparticle structure.
  • This approach enables independent tuning of crystallite and particle size, expanding synthesis boundaries.
  • The platform is applicable to a broad range of nanoparticle synthesis processes.