Block Copolymer-Directed\nSingle-Diamond Hybrid Structures\nDerived from X‑ray Nanotomography

Block copolymers are recognized as a valuable platform\nfor creating\nnanostructured materials. Morphologies formed by block copolymer self-assembly\ncan be transferred into a wide range of inorganic materials, enabling\napplications including energy storage and metamaterials. However,\nimaging of the underlying, often complex, nanostructures in large\nvolumes has remained a challenge, limiting progress in materials development.\nTaking advantage of recent advances in X-ray nanotomography, we noninvasively\nimaged exceptionally large volumes of nanostructured hybrid materials\nat high resolution, revealing a single-diamond morphology in a triblock\nterpolymer–gold composite network. This morphology, which is\nubiquitous in nature, has so far remained elusive in block copolymer-derived\nmaterials, despite its potential to create materials with large photonic\nbandgaps. The discovery was made possible by the precise analysis\nof distortions in a large volume of the self-assembled diamond network,\nwhich are difficult to unambiguously assess using traditional characterization\ntools. We anticipate that high-resolution X-ray nanotomography, which\nallows imaging of much larger sample volumes than electron-based tomography,\nwill become a powerful tool for the quantitative analysis of complex\nnanostructures and that structures such as the triblock terpolymer-directed\nsingle diamond will enable the generation of advanced multicomponent\ncomposites with hitherto unknown property profiles.