It is the purpose of this study to obtain the foundamental information of non-stoichiometric PZT powders in the pulverizing process by wet method. The effects of wet pulverizing by ball-milling (for 150 hrs.) on the structural properties of the powders have been studied by thermobalance, X-ray diffraction and some other methods.
The following results were obtained.
(1) The weight of the specimens pulverized for a long time decreased continuously up to 900°C, due to the discharge of the bonding water caused by the mechano-chemical reaction between PZT and water by wet pulverizing.
(2) The crystallite dimension of the powder decreased remarkably for 25-50 hours. The lattice distortion, however, increased gradually with decreasing the crystallite dimension and this was not recovered to the original stage by heating up to 900°C for the specimen pulverized for 150 hours.
(3) The layer of the bonding water penetrated gradually to the inner part of grains from the surface with increasing of the pulverizing time. From this result, it was found that the unfarorable effects on the properties of PZT appeared by such a long pulverizing time.
(4) As a result of calculating the number of OH radical by assuming that the weight loss at 150-900°C is due to the bonding water, the number of OH radical increased with increasing of the pulverizing time, and it attained nearly constant values after 100 hours.
(5) Judging from the above mentioned results, the bonding water seemed to be not only the adsorbed water on the surface of PZT particles but also the water which penetrated into PZT grains, and formed the hydrogen bonding with the parts of oxygen ion.
(6) After the long time pulverizing, the aggregation or agglomeration of the primary particles occurred and resulted in the growth of the secondary particles.
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