Solid-solution method for producing iron-containing active materials for rechargeable oxide-ion battery cells
View Patent ↗The present invention describes a solid-solution synthesis method for producing porous Fe-containing active material ( 74 ) wherein Fe is interwoven with supporting oxide(s) by the following steps: mixing ( 64 ) Fe-containing specie (α) ( 60 ) and a supporting specie (β) ( 62 ) containing element of X, to provide a mixture ( 66 ), high-temperature treatment ( 68 ) to provide a Fe—X—O solid solution ( 70 ), and reducing ( 72 ) the solid solution to provide the Fe-containing active material wherein Fe is interwoven with X oxide(s) ( 74 ).
1. A solid-solution method for producing an iron-containing active material to be used in a metal electrode of a rechargeable oxide-ion battery cell comprising the steps:
i) providing iron-containing specie (α);
ii) providing supporting specie (β) containing an element of X, where X is not iron;
iii) mixing the Fe-containing specie (α) and the supporting specie (β) to produce a α+β mixture;
iv) subjecting the mixture to a high temperature treatment for a period of time effective to produce a solid solution of Fe—X—O, where Fe and X are homogeneously distributed at the microscopic level; and
v) reducing the solid solution of Fe—X—O to provide metallic Fe interwoven with X oxide(s), where the reduction causes loss of oxygen to produce porous Fe-containing active material.
2. The method of claim 1 , wherein the Fe-containing specie (α) of step i is in the form of solid, liquid, or solid-liquid mixture.
3. The method of claim 1 , wherein the supporting specie (β) of step ii is in the form of solid, liquid, or solid-liquid mixture.
4. The method of claim 1 , wherein the supporting specie (β) of claim 3 is selected from X oxide, X halide, X nitrate, and X carbonate.
5. The method of claim 1 , wherein the supporting specie (β) contains element X selected from the group consisting of Li, Na, K, Mg, Ca, Sr, Ba, Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Al, Ga, Y, Nb, Mo, Ru, W, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
6. The method of claim 1 , wherein the supporting species (β) containing element X is selected from the group consisting of Ca, Sr, Ba, Sc, Ti, V, Mn, Co, Ni, Y, Nb, Ru, W, and La.
7. The method of claim 1 , wherein the ratio of X/(X+Fe), in terms of molar number, varies from 0.001 to 0.6.
8. The method of claim 1 , wherein mixing the Fe-containing specie (α) and the supporting specie (β) of step iii comprises at least one of blending, milling, and solution approaches.
9. The method of claim 1 , wherein the high temperature treatment of step iv is conducted in the temperature between 500° C. and 2,500° C.
10. The method of claim 1 , wherein the reducing environment of step v involves heating at the temperatures between 400° C. and 1200° C. in a reducing gas selected from N 2 —H 2 , H 2 —H 2 O, CO—CO 2 , and mixtures thereof.
11. The method of claim 10 , wherein the final, reduced Fe particle size ranges from 0.001 micrometers to 100 micrometers.
12. The method of claim 10 , wherein the final porosity of the Fe-containing material in step v is from 10 vol. % to 70 vol. %, preferably 25 vol. % to 50 vol. %.