Instant One‐Pot Preparation of Functional Layered Double Hydroxides (LDHs) via a Continuous Hydrothermal Approach

Abstract Instant one‐pot synthesis of functional layered double hydroxides (LDHs) is demonstrated for the first time using a continuous hydrothermal multi‐step process. The as‐prepared pristine material displays high crystallinity and very small LDH nanoparticle size, lateral dimensions below 100 nm and a thickness below 20 nm, all being achieved in only 5 s. This approach was extended to the preparation of i) pristine LDH with different compositions by varying the cation (Mg, Ni, or Zn) and the anion (CO₃, NO₃) and ii) functional LDH by varying the functionalization agent, for example long organic molecules (hybrid LDH), enzymes (bio‐hybrid LDH) or inorganic metal/oxide nanocrystals (inorganic‐LDH). Beyond the design of functional LDH, this paper presents proof of concept for a continuous, one‐pot and multistep high temperature/high pressure (HT/HP) process for the assembly of nanoscaled materials.