All-silica zeolite DDR was prepared by microwave-aided hydrothermal synthesis and characterized by X-ray diffraction, scanning electron microscopy, infra-red spectroscopy, nitrogen adsorption , elemental analysis and thermal gravimetric analysis . Microwave-aided heating significantly reduced the synthesis time from 25 d to 3 d and crystal size from 8 μm to 2 μm. With the help of seeding, the synthesis time and crystal size were further reduced to 6 h and 0.7 μm respectively. The crystal size decreased with seed content. The fragmentation of seed crystals had positive impact on reducing crystal size and increasing product yield. The aging of mother liquor and decrease of H 2 O/SiO 2 had little impact on crystal size.
Transparent nanoceramics embedded with highly dense crystalline domains are promising for applications in missile guidance, infrared night vision, and laser and nuclear radiation detection. Unfortunately, current nanoceramics are strictly constrained by the stringent construction procedures such as super-high pressure and containerless processing. Here, a pressureless crystallization engineering strategy in glass for elaboration of transparent nanoceramics and fibers is proposed and experimentally demonstrated. By intentional creation of a sharp contrast between nucleation and growth rates, the crystal growth rate during glass crystallization can be significantly suppressed. Importantly, this unique phase-transition habit enables the achievement of transparent nanoceramics and even smooth fibers with extremely tiny crystalline size (≈20 nm) and high crystallinity (≈97%) under atmospheric pressure. This allows the generation of an attractive nonlinear optical response such as dynamic optical filtering and luminescence in the mid-infrared waveband of 4300–4950 nm. These findings highlight that the strategy to switch the phase-transition habit of glass into the unconventional crystallization regime may provide new opportunities for the creation of next-generation nanoceramics and fibers.