Phase-pure lithium aluminium titanium phosphate and method for its production and its use
View Patent ↗The present invention relates to a method for producing lithium aluminum titanium phosphates of the general formula Li 1+x Ti 2−x Al x (PO 4 ) 3 , wherein x is ≦0.4, a method for their production as well as their use as solid-state electrolytes in lithium ion accumulators.
1. A method for producing a phase-pure lithium aluminum titanium phosphate of the formula Li 1+x Ti 2−x Al x (PO 4 ) 3 comprising the steps of:
a) providing an aqueous liquid phosphoric acid,
b) adding a mixture of a lithium compound, titanium dioxide and an oxygen-containing aluminum compound to the aqueous phosphoric acid of step a),
c) heating the mixture of step b) in order to obtain a solid intermediate product, and
d) calcining the solid intermediate product of step c), wherein x is ≦0.4 and >0, and the concentration of magnetic metals and magnetic metal compounds of the elements Fe, Cr and Ni in the phase-pure lithium aluminum titanium phosphate is ≦1 ppm.
2. The method according to claim 1 , wherein the aqueous liquid phosphoric acid is aqueous liquid orthophosphoric acid.
3. The method according to claim 1 , wherein lithium carbonate is used as lithium compound.
4. The method according to claim 1 , wherein Al(OH) 3 is used as oxygen-containing aluminum compound.
5. The method according to claim 1 , wherein the step of heating is carried out at a temperature of from 200 to 300° C.
6. The method according to claim 5 , wherein the calcining takes place at a temperature in the range from 850° C. to 1000° C.
7. The method according to claim 6 , wherein the calcining is carried out over a period of from 5 to 24 hours.
8. The method according to claim 1 , wherein a stoichiometric excess of lithium compound is used in step b).
9. A method for producing a phase-pure lithium aluminum titanium phosphate of the formula Li 1+x Ti 2−x Al x (PO 4 ) 3 comprising the steps of:
a) providing 85% orthophosphoric acid,
b) adding a mixture of a lithium compound, titanium dioxide and an oxygen-containing aluminum compound to the 85% orthophosphoric acid of step a),
c) heating the mixture of step b) in order to obtain a solid intermediate product, and
d) calcining the solid intermediate product of step c),
wherein x is ≦0.4 and >0, and the concentration of magnetic metals and magnetic metal compounds of the elements Fe, Cr and Ni in the phase-pure lithium aluminum titanium phosphate is ≦1 ppm.
10. The method according to claim 9 , wherein lithium carbonate is used as lithium compound.
11. The method according to claim 9 , wherein Al(OH) 3 is used as oxygen-containing aluminum compound.
12. The method according to claim 9 , wherein the step of heating is carried out at a temperature of from 200 to 300° C.
13. The method according to claim 12 , wherein the calcining takes place at a temperature in the range from 850° C. to 1000° C.
14. The method according to claim 13 , wherein the calcining is carried out over a period of from 5 to 24 hours.
15. The method according to claim 9 , wherein a stoichiometric excess of lithium compound is used in step b).