Abstract
Achieving precise control of materials synthesis is a cornerstone of modern manufacturing, driving efficiency, functionality, and device innovation. This review examines the roles of in situ transmission electron microscopy (TEM) and neutron scattering (NS) in advancing our understanding of these processes. In situ TEM offers atomic-scale insights into nucleation, growth, and phase transitions, while NS provides an analysis of reaction pathways, phase evolution, and structural transformations over broader length scales. Recent advancements in hardware have greatly improved spatial, temporal, and environmental control in in situ experiments. TEM enables breakthroughs in thermally controlled synthesis, gas-phase deposition, and beam-induced fabrication, including single-atom device creation. NS, particularly in situ neutron diffraction and imaging, are essential for studying bulk-level synthesis pathways. Together, these techniques offer a multiscale view of synthesis and processing. Integrating artificial intelligence (AI), automated workflows, and multimodal characterization is highlighted as a path toward high-throughput, predictive synthesis. By discussing challenges and opportunities in instrumentation and analysis, this review proposes a multiscale approach to accelerate innovation in materials synthesis, with applications across energy storage, quantum materials, and next-generation manufacturing.
| Original language | English |
|---|---|
| Pages (from-to) | 8731-8763 |
| Number of pages | 33 |
| Journal | Chemical Reviews |
| Volume | 125 |
| Issue number | 18 |
| DOIs | |
| State | Published - Sep 24 2025 |
Funding
This work was supported by the U.S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Materials Sciences and Engineering (H.K.). M.C. acknowledges support from Energy Storage Research Alliance (ESRA, DE-AC02-06CH11357), an Energy Innovation Hub funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences. Y.C. and K.A. were supported by the High Flux Isotope Reactor and the Spallation Neutron Source, DOE Office of Science User Facilities operated by Oak Ridge National Laboratory (ORNL). Some figures are based on experiments conducted at the Center for Nanophase Materials Sciences (CNMS), a U.S. DOE Office of Science User Facility at ORNL. K.R. acknowledges support from the Miller Institute for Basic Research in Science. The authors thank Frances M. Ross for valuable discussions.