The reproducible fabrication of nanostructured 3Dimensional (3D) binary colloidal crystal (bCC) in a defined geometric space through a simple one step process is detailed. This method allows for the potential fabrication of a bCC in a sealed mu chip within a defined area or channel by capillary forces, unlike other bCC formation methods such as dip-drawing, where the substrate must be submerged in a suspension to form a bCC, or bCC monolayers, which are fabricated at the water air interface. Through simple variation in volume fraction ratio (VFS/L) of nano-(denoted small, S) and macro-sized (denoted large, L) polystyrene (PS) spheres and diameter size ratio (D-S/L), the manipulation of bCC structures was also achieved. Variation of nano-sized PS sphere number within the interstitial voids formed between neighbouring macro-sized spheres enabled the reproducible fabrication of LS2 and LS6 structures, which contain I and 3 nano-spheres respectively in each interstitial void. It must be noted that while VFS/L allows for control of the final LSn structure, thickness of bCC formation in this manner is independent of VFS/L. (C) 2014 Elsevier Inc. All rights reserved.