A novel method was proposed to prepare boron trifluoride diethyl etherate ((C2H5)(2)O center dot BF3)-loaded microcapsules. To protect the high activity of (C2H5)(2)O center dot BF3, hollow microcapsules were prepared via UV-initiated polymerization in emulsion with the aid of CO2 microbubble templates, evacuation, and immersion in (C2H5)(2)O center dot BF3 allowing infiltration of the chemical. The selected photo-initiator induced rapid curing of the oil layer in the CO2/oil/water emulsion, ensuring production of the desired hollow capsules. Structure, geometry, morphology and properties of the resultants were carefully studied in relation to their synthesis conditions and loading behavior in liquid (C2H5)(2)O center dot BF3. The results indicated that the amount of(C2H5)(2)O center dot BF3 filled in the capsules can be adjusted by changing the shell composition. Having been encapsulated, (C2H5)(2)O center dot BF3 maintained its reactivity with epoxy. (C) 2008 Elsevier Ltd. All rights reserved.