Method for preparing electroconductive mayenite type compound
View Patent ↗Provided is a method for preparing an electroconductive mayenite type compound with good properties readily and stably at low cost without need for expensive facilities, a reaction at high temperature and for a long period of time, or complicated control of reaction. A method for preparing an electroconductive mayenite type compound comprises a step of subjecting a precursor to heat treatment, wherein the precursor contains Ca and/or Sr, and Al, a molar ratio of (a total of CaO and SrO:Al 2 O 3 ) is from (12.6:6.4) to (11.7:7.3) as calculated as oxides, a total content of CaO, SrO and Al 2 O 3 in the precursor is at least 50 mol %, and the precursor is a vitreous or crystalline material; and the method comprises a step of mixing the precursor with a reducing agent and performing the heat treatment of holding the mixture at 600-1,415° C. in an inert gas or vacuum atmosphere with an oxygen partial pressure of at most 10 Pa.
1. A method for preparing an electroconductive compound, which comprises a step of subjecting a precursor to heat treatment,
wherein
the precursor contains CaO and/or SrO, and Al 2 O 3 ,
the molar ratio of a total of CaO and SrO:Al 2 O 3 is from 12.6:6.4 to 11.7:7.3 as calculated as oxides,
the total content of CaO, SrO and Al 2 O 3 in the precursor is at least 50 mol %, and
the precursor is a vitreous or crystalline material; and
wherein the heat treatment is carried out by holding a mixture of the precursor and a reducing agent at 600-1,415° C. in an inert gas or vacuum atmosphere with an oxygen partial pressure of at most 10 Pa, where the reducing agent is selected from the group consisting of a metal, an intermetallic compound and a metallic compound.
2. The method according to claim 1 , wherein the precursor is
a mayenite compound having a composition of 12CaO.7Al 2 O 3 and having a crystal structure composed of three-dimensionally linked voids, or
an isomorphous compound obtained by replacing part of Ca and Al in 12CaO.7Al 2 O 3 with another element.
3. The method according to claim 1 , wherein part of Al contained in the precursor is replaced by the same number of Si atoms or Ge atoms.
4. The method according to claim 1 , wherein the precursor contains
from 0 to 17 mol % in total of at least one member selected from the group consisting of Si, Ge and B, as calculated as oxides;
from 0 to 5 mol % in total of at least one member selected from the group consisting of Li, Na and K, as calculated as oxides;
from 0 to 10 mol % in total of at least one member selected from the group consisting of Mg and Ba, as calculated as oxides; and
from 0 to 8 mol % in total of at least one rare earth element and at least one transition metal element, where the at least one rare earth element is selected from the group consisting of Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm and Yb and the at least one transition metal element is selected from the group consisting of Ti, V, Cr, Mn, Fe, Co, Ni and Cu, as calculated as oxides.
5. The method according to claim 1 , wherein the precursor and the reducing agent are powders with an average particle size of at most 100 μm.
6. The method according to claim 5 , wherein the powder of the reducing agent is a powder of a metal.
7. The method according to claim 6 , wherein the metal is aluminum and the inert gas contains at least Ar or He.
8. The method according to claim 4 , wherein the precursor contains from 3 to 17 mol % in total of at least one member selected from the group consisting of Si, Ge and B, as calculated as oxides.