Facile Salt-Assisted Hydrothermal Synthesis of Nanodiamonds from CHO Precursors: Atomic-Scale Mechanistic Insights

TL;DR

This study demonstrates a sustainable hydrothermal method for synthesizing nanodiamonds from CHO precursors, revealing atomic-scale mechanisms and factors influencing their structure, with implications for advanced technological applications.

Contribution

It provides detailed atomic-scale insights into diamond formation mechanisms during hydrothermal synthesis using various CHO-based precursors.

Findings

Diamond-specific lattice planes confirmed by microscopy.

Precursor type and ionic composition influence defect patterns.

Atomic imaging reveals graphite-to-diamond transition mechanisms.

Abstract

Hydrothermal synthesis offers an economical and scalable way to produce nanodiamonds under relatively mild, low-pressure and low-temperature conditions. However,its sustainability and the detailed mechanisms behind diamond formation in such environments are still not fully understood. In this work, we designed ten hydrothermal synthesis protocols using different CHO-based molecular precursors containing COOH and OH groups, such as organic acids, polyols, sugars, and polysaccharides.The reactions were carried out at 190 degrees Centigrade in chlorinated, strongly alkaline aqueous solutions with alkali and alkaline-earth metal ions. Using high-resolution transmission electron microscopy and X-ray photoelectron spectroscopy, we confirmed the presence of diamond-specific lattice planes and sp3-hybridized carbon structures. Our results show that the type of precursor, its molecular size, and the ionic composition of the solution play key roles in determining the defect patterns and polymorph distribution in the resulting nanodiamonds. Atomic-scale imaging showed both coherent and incoherent transitions from graphite to diamond, along with gradual lattice compression and complex twinning patterns. These observations provide direct insight into how interfacial crystallography and defect dynamics drive diamond formation in aqueous systems. Overall, the study positions hydrothermal synthesis as a sustainable, chemistry-driven, and tunable approach for creating nanodiamonds tailored for applications in quantum technologies, biomedicine, catalysis, and advanced materials.