Homogeneous precipitation method using urea was applied to the preparation of calcium phosphates. Acidic-aqueous solutions (0.5 mol·dm
-3 HNO
3 500cm
3) containing 0.167 mol·dm
-3 Ca (NO
3)
2, 0.1 mol·dm
-3 (NH
4)
2HPO
4 (Ca/P=1.67) and 0.5 mol·dm
-3 (NH
2)
2CO were refluxed respectively at 80, 90, 95 and 100 °C for various lengths of time. The pH of each solution was measured continuously during the reaction. The products were characterized by X-ray powder diffractometry, IR spectroscopy, SEM and TG. During the reaction, two morphologies of the products were formed and separated into two layers at the initial stage; agglomerates of particles of dicalcium phosphate anhydrate (CaHPO
4) at the bottom of the flask and fibrous octacalcium phosphate [Ca
8H
2 (PO
4)
6·5H
2O, OCP] in the upper solution. After the reaction finished, both products changed completely into apatite containing CO
32- (CO
3Ap).
The other results were as follows :
(1) A mixture of whisker-like CO
3Ap and fibrous CO
3Ap was obtained under the reaction conditions of 100°C-17h and 95°C-47h and 90°C-80h, the fibrous OCP was also obtained at 80°C-22h. The CO
3Ap was formed with the hydrolysis of CaHPO
4 and OCP, which both precipitated at the initial stage.
(2) By heating up to 1200°C in air, the CO
3Ap obtained at 95°C-47h and 90°C-80h changed into hydroxyapatite [Ca
10 (PO
4)
6 (OH)
2, HAp], losing CO
2. The CO
3Ap obtained at 100°C-17h changed into the mixture of HAp and α-tricalcium phosphate [α-Ca
3 (PO
4)
2, α-TCP] by heating. Even after the heating, the HAp had whisker-like or fibrous morphology. However, the OCP fiber shrank and showed partially sinterability due to the heating.
(3) The flexible sheets and porous compacts of CO
3Ap and OCP were obtained.
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