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Annual Report 2009/2010 - JUWEL - Forschungszentrum Jülich

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The morphology of the powder was studied with scanning electron microscopy (SEM) as<br />

shown in Fig. 58. The rhabdophane particles were round and their diameters is between 0.1<br />

and 2 <br />

Since the phase transformation (hexagonal to monoclinic) ends around 850 °C, the<br />

rhabdophane particles were heated up to 1000 °C, where they consolidate together. This is<br />

the beginning of the sintering process. The comparison between the left and the right photo<br />

in Fig. 58 shows significantly the beginning of the densification.<br />

Fig. 58: SEM images of LaPO 4 . 0.5H 2 O sample (left) and of calcined (1000°C) LaPO 4 . 0.5 H 2 O<br />

sample (right).<br />

In this work, leaching tests are planned to be done on both powder and pellets. Indeed<br />

leaching tests on pellets is a standard method (e.g. Soxhlet method) and a study on pellet<br />

density is necessary.<br />

The investigated powders were compacted by cold uniaxial pressing, applying pressures<br />

between 130 and 510 MPa. The pellets were made by powder prepared by hydrothermal<br />

synthesis. The relative green density and the relative sintered density both depend on the<br />

applied pressure (Fig. 59). The results of the relative green density in relation to the<br />

logarithm of the pressure show that the values form a linear function. This is a typical<br />

behaviour for ceramic materials [6]. After the sintering at 1400°C [7], the relative sintered<br />

density of the pellets was determined by Archimedes method, i.e. by hydrostatic weighing in<br />

water (see lower figure).<br />

The value of the pressure related to the maximal density - optimal pressure - is between 250<br />

and 400 MPa. The sintered density at this optimal pressure is above 98% of theoretical<br />

density.<br />

85

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