The sequence of reactions that occur during the synthesis of (Hg,Bi)Ba
2Ca2Cu3Oy (HgBi1223) was studied using a series of quenching experimen
ts. The formation and decomposition of the intermediate phases during
the high temperature reaction were followed as a function of temperatu
re. Heat treatment conditions were optimized for the synthesis of pure
HgBi1223 phase using commercial BaCaCuO precursor powders. An additio
nal lower temperature annealing stage after high temperature reaction
is shown to improve the microstructural characteristics of HgBi1223 sa
mples. Control of Hg-pressure is shown to be crucial for achieving gra
in growth and texture in the final products. A novel approach for the
control of HE-pressure during the synthesis of HgBi1223, which consist
s of using CaHgO2 as an 'external Hg-source', is demonstrated. Samples
synthesized using the new synthesis protocol exhibit improved microst
ructural and magnetization properties. (C) 1998 Elsevier Science B.V.