Adsorbent material and method for producing crystalline silicotitanate
US-9486776-B2 · Nov 8, 2016 · US
US8992795B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-8992795-B2 |
| Application number | US-201113273262-A |
| Country | US |
| Kind code | B2 |
| Filing date | Oct 14, 2011 |
| Priority date | Oct 15, 2010 |
| Publication date | Mar 31, 2015 |
| Grant date | Mar 31, 2015 |
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In a manufacturing process of a positive electrode active material for a power storage device, which includes a lithium silicate compound represented by a general formula Li 2 MSiO 4 , heat treatment is performed at a high temperature on a mixture material, grinding treatment is performed, a carbon-based material is added, and then heat treatment is performed again. Therefore, the reactivity between the substances contained in the mixture material is enhanced, favorable crystallinity can be obtained, and further microparticulation of the grain size of crystal which is grown larger by the high temperature treatment and crystallinity recovery are achieved; and at the same time, carbon can be supported on the surfaces of particles of the crystallized mixture material. Accordingly, a positive electrode active material for a power storage device, in which electron conductivity is improved, can be manufactured.
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What is claimed is: 1. A method for manufacturing a positive electrode active material for a power storage device, comprising the steps of: performing first heat treatment on a first mixture material in which a compound containing lithium, a compound containing a transition metal, and a compound containing silicon are mixed to obtain first particles; performing first mixing treatment on the first particles to obtain second particles after the first heat treatment; performing second heat treatment on the second particles at a temperature higher than a temperature of the first heat treatment to obtain third particles; performing grinding treatment on the third particles to obtain fourth particles after the second heat treatment; adding a carbon-based material to the fourth particles and performing second mixing treatment to obtain a second mixture; and performing third heat treatment on the second mixture at a temperature lower than a temperature of the second heat treatment to obtain fifth particles, wherein the grinding treatment is performed by a planetary ball mill after adding a solvent to the second particles, wherein the grinding treatment is performed for longer time than the first mixing treatment, wherein an average primary particle size of the fifth particles is smaller than that of the third particles, and wherein each of the first particles, the second particles, the third particles, the fourth particles, and the fifth particles comprises lithium metal silicate. 2. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein the transition metal is selected from the group consisting of manganese, iron, cobalt, and nickel. 3. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein the first heat treatment is performed at a temperature of higher than or equal to 650° C. and lower than or equal to 1000° C., wherein the second heat treatment is performed at a temperature of higher than or equal to 800° C. and lower than or equal to 1500° C., and wherein the third heat treatment is performed at a temperature of higher than or equal to 400° C. and lower than or equal to 900° C. 4. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein the carbon-based material is selected from the group consisting of glucose, cyclic monosaccharide, straight-chain monosaccharide, and polysaccharide. 5. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein a thickness of a carbon layer supported on a surface of each of the third particles is less than or equal to 100 nm. 6. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein each of the average primary particle size of the first particles and that of the third particles is measured with a SEM. 7. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein the third particles have a first crystallinity, wherein the fourth particles have a second crystallinity, wherein the fifth particles have a third crystallinity, wherein the second crystallinity is lower than the first crystallinity, and wherein the second crystallinity is lower than the third crystallinity. 8. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein the first mixing treatment is performed by a planetary ball mill. 9. The method for manufacturing a positive electrode active material for a power storage device, according to claim 8 , wherein the first mixing treatment is performed for 30 minutes and shorter than or equal to 5 hours, and wherein the grinding treatment is performed for longer than or equal to 10 hours and shorter than or equal to 60 hours. 10. The method for manufacturing a positive electrode active material for a power storage device, according to claim 1 , wherein the fifth particles comprise lithium metal silicate represented by Formula Li 2 MSiO 4 , and wherein M is selected from the group consisting of manganese, iron, cobalt, and nickel. 11. A method for manufacturing a positive electrode active material for a power storage device, comprising the steps of: performing first heat treatment on a mixture material in which a compound containing lithium, a compound containing a transition metal, and a compound containing silicon are mixed to obtain first particles; performing mixing treatment on the first particles to obtain second particles after the first heat treatment; performing second heat treatment on the second particles at a temperature higher than a temperature of the first heat treatment to obtain third particles; performing grinding treatment on the third particles to obtain fourth particles after the first heat treatment; and performing third heat treatment at a temperature lower than a temperature of the first heat treatment on the fourth particles to obtain fifth particles, wherein the grinding treatment is performed by a planetary ball mill after adding a solvent to the third particles, wherein the grinding treatment is performed for longer time than the mixing treatment, wherein an average primary particle size of the fifth particles is smaller than that of the third particles, and wherein each of the first particles, the second particles, and the third particles comprises lithium metal silicate. 12. The method for manufacturing a positive electrode active material for a power storage device, according to claim 11 , wherein the transition metal is selected from the group consisting of manganese, iron, cobalt, and nickel. 13. The method for manufacturing a positive electrode active material for a power storage device, according to claim 11 , wherein the first heat treatment is performed at a temperature of higher than or equal to 650° C. and lower than or equal to 1000° C., wherein the second heat treatment is performed at a temperature of higher than or equal to 800° C. and lower than or equal to 1500° C., and wherein the second third heat treatment is performed at a temperature of higher than or equal to 400° C. and lower than or equal to 900° C. 14. The method for manufacturing a positive electrode active material for a power storage device, according to claim 11 , wherein a thickness of a carbon layer supported on a surface of the positive electrode active material is less than or equal to 100 nm. 15. The method for manufacturing a positive electrode active material for a power storage device, according to claim 11 , wherein each of the average primary particle size of the first particles and that of the third particles is measured with a SEM. 16. The method for manufacturing a positive electrode active material for a power storage device, according to claim 11 , wherein the third particles have a first crystallinity, wherein the fourth particles have a second crystallinity, wherein the fifth particles have a third crystallinity, wherein the second crystallinity is lower than the first crystallinity, and wherein the second crystallinity is lower than the third crystallinity. 17. The method for manufacturing a positive electrode active material for a power storage device, according to claim 11 , wherein the mixing treatment to obtain the second particles is performed by a planetary ball mill. 18
Energy storage using batteries · CPC title
Silicates (persilicates C01B15/14 {; containing aluminium C01B33/26}) · CPC title
Li-accumulators · CPC title
as layered products · CPC title
involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title
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