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14 декабря, 2021
Pellet or block fabrication makes use of proven technologies in the ceramic industry. Pressing and sintering of ceramic powders is a widely used and cost-effective industrial process. Pellets and rectangular blocks can be manufactured up to some centimeters in size with excellent material homogeneity and controlled density. Thus, LiAlO2, Li2ZrO3, and Li2TiO3 pellets meeting dimensional, microstructural, and purity characteristics were produced by Pechiney in collaboration with CEA.52 Similar results were obtained by ENEA, SCK/CEN, UKAEA- Springfields, and US laboratories.65,73-75
Kapychev et a/.30 fabricated pellets of Li4SiO4, metasilicate (Li2SiO3), and aluminate (LiAlO2), with a diameter of about 10 mm and heights of 5, 10, and 14 mm.
For TBR considerations, the density of the pebbles should be high and enable a dense packing to achieve a high lithium density. Further comments on pebble shapes are given in a later section. The presently used or developed processes are as follows:
1. A melting-spraying process was used at KIT (formerly FZK), in collaboration with Schott Glas — werke, for the production of 0.25-0.63 mm Li4SiO4 and Li4SiO4-SiO2 pebbles76 (see Figure 11). After annealing, spherical pebbles of 95-96% of theoretical density (TD) exhibiting satisfactory mechanical strength were obtained. Long-term annealing experiments on various candidates ceramic breeder materials were performed by Piazza et a/.77 An alternative route avoiding use of carbonate and using hydroxide was developed by Knitter et a/.,78 with slightly lower density. The reference composition is Li4SiO4 + 2.5 wt SiO2, resulting in a two-phase Li4SiO4 + Li6Si2O7 structure in as-melted condition, and Li4SiO4 + Li2SiO3 after heat treatment (see Figure 12).
A melting-dropping process was investigated by Tsuchiya et a/.79 in collaboration with Mitsubishi to produce 1-mm Li2O spheres.
2. Sol-gel type processes were developed at Japan Atomic Energy Agency (JAEA), with Nuclear Fuel Industries, to produce 1 mm Li2O and 1.6 mm Li2TiO3 pebbles80 (see Figure 13). Similarly, Muis and coworkers81 at Energy Research Centre of The Netherlands (ECN) produced 0.5-1.0mm Li2TiO3
Figure 11 Illustration of the melt drop and jet spraying processes developed for production of Li4SiO4 pebbles at KIT. Reproduced from Kolb, M. H. H.; Knitter, R.; Kaufmann, U.; Mundt, D. Fusion Eng. Des. 2011, doi: 10.1016/j. fusengdes.2011.01.104. |
pebbles. In these cases, the pebble densities were <80% TD. Further work led to pebbles with Li2TiO3 + 5% TiO2 composition82 (see Figure 14).
Wu et a/.83 started the development of a sol-gel type process for Li4SiO4 and achieved 75% of TD for 1.2 mm diameter pebbles.
3. A process consisting of extrusion, spheronization, and sintering has, for several years, been used by AECL to produce 1.2 mm LiAlO2, Li2ZrO3, and Li2TiO3 pebbles in collaboration with Ceramics Kingston.3 Material densities are in the 80-90% TD range.
Similar process trials were made by Lulewicz and Roux53 at CEA, with Pechiney, to produce 1 mm Li2ZrO3 pebbles, and later work concerned Li2TiO384,193 (Figure 15).
4. An agglomeration-sintering process has been used by JAEA, in collaboration with Kawasaki Industries,
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Li2TiO3 solvent (H2°2 etc.) Dissolving (binder) (mixing) „ , t. In air |
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Gelation solvent Dropping |
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Heating Calcination sintering |
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ECN SEI 15.0kV x50 100ptm WD36mm
Figure 15 Scanning electron micrographs of L12T1O3 pebbles produced by an extrusion-spheronization method (see text).
for producing 1 mm Li2O, Li4SiO4, and Li2ZrO3 pebbles. Pebble densities in the 90% TD range were obtained.85 This process has also been investigated at CEA for producing 1 mm Li2TiO3 pebbles. Pebble density of 90% TD and good mechanical strength were obtained.84
5. Zhu et al. developed a wet process for fabrication of Li3TaO4 ceramic pebbles. Typical pebble diameters are about 0.7-1.0mm, and the density achieved is over 90% TD, with crush loads more than 40 N.56 X-ray diffraction (XRD) patterns showed 99% of p-Li3TaO4 and traces of LiTaO3.
The necessity to recycle ceramic breeders after service imposes specific requirements on pebble manufacturing technologies. This reprocessing aspect may become a significant driver in fusion power economics on a longer term. See Sections 4.15.7 and 4.15.8.8 for further discussion.