Sulfide glass and crystalline solid electrolyte production method, crystalline solid electrolyte, sulfide glass and solid-state battery
A method for producing sulfide glass wherein phosphorus sulfide satisfying the following formula (1) is used as a raw material: 100× A/B ≥37 (1) wherein in the formula, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
1. A method comprising producing sulfide glass from a raw material comprising phosphorus sulfide satisfying a formula (1):
100× A/B≥ 37 (1)
wherein in the formula, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
2. A method comprising producing sulfide glass from a raw material comprising phosphorus sulfide satisfying a formula (2):
37≤100×( A+D )/ B ≤70 (2)
wherein in the formula, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, D is peak areas of peaks that appear at peak positions in a range of 84.0 ppm or more and 86.0 ppm or less, and 110 ppm or more and 113 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
3. The method of claim 1 , wherein the phosphorus sulfide further satisfies a formula (2):
37≤100×( A+D )/ B ≤70 (2)
wherein in the formula, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, D is peak areas of peaks that appear at peak positions in a range of 84.0 ppm or more and 86.0 ppm or less, and 110 ppm or more and 113 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
4. The method of claim 1 , wherein the phosphorus sulfide further satisfies formulas (3) and (4):
37≤100× A/B≤ 60 (3)
25≤100× C/B≤ 60 (4)
wherein in the formulas, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, C is peak areas of peaks that appear in a range of 56.6 ppm or more and 57.1 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
5. The method of claim 1 , wherein the phosphorus sulfide further satisfies formulas (3), (4) and (5):
37≤100× A/B≤ 60 (3)
25≤100× C/B≤ 60 (4)
0≤100× D/B≤ 10 (5)
wherein in the formulas, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, C is peak areas of peaks that appear in a range of 56.6 ppm or more and 57.1 ppm or less in 31 PNMR spectroscopy, and D is peak areas of peaks that appear in a range of 84.0 ppm or more and 86.0 ppm or less, and 110 ppm or more and 113 ppm or less, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
6. The method of claim 3 , wherein the phosphorus sulfide further satisfies formulas (3), (4) and (5):
37≤100× A/B≤ 60 (3)
25≤100× C/B≤ 60 (4)
0≤100× D/B≤ 10 (5)
wherein in the formulas, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, C is peak areas of peaks that appear in a range of 56.6 ppm or more and 57.1 ppm or less in 31 PNMR spectroscopy, and D is peak areas of peaks that appear in a range of 84.0 ppm or more and 86.0 ppm or less, and 110 ppm or more and 113 ppm or less, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
7. The method of claim 1 , wherein the phosphorus sulfide further satisfies formulas (3) and (6):
37≤100× A/B≤ 60 (3)
0.1≤100× D/B≤ 10 (6)
wherein in the formulas, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, D is peak areas of peaks that appear in a range of 84.0 ppm or more and 86.0 ppm or less, and 110 ppm or more and 113 ppm or less, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
8. The method of claim 1 , wherein the phosphorus sulfide further satisfies a formula (3), and the raw material further comprises lithium sulfide:
37≤100× A/B≤ 60 (3)
wherein in the formulas, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
9. The method of claim 8 , wherein the raw material further comprises a lithium halide.
10. The method of claim 9 , wherein the raw material is mixed in a solvent.
11. The method of claim 10 , wherein the solvent is a hydrocarbon solvent.
12. The method of claim 1 , wherein the phosphorus sulfide further satisfies a formula (3), and the raw material is mixed in a solvent:
37≤100× A/B≤ 60 (3)
wherein in the formulas, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
13. The method of claim 3 , wherein the raw material further comprises lithium sulfide and a lithium halide.
14. The method of claim 13 , wherein the raw material is mixed in a solvent.
15. The method of claim 2 , wherein the phosphorus sulfide further satisfies formula (4):
25≤100× C/B≤ 60 (4)
wherein in the formula, C is peak areas of peaks that appear in a range of 56.6 ppm or more and 57.1 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.
16. The method of claim 2 , wherein the raw material further comprises lithium sulfide.
17. The method of claim 16 , wherein the raw material further comprises a lithium halide.
18. The method of claim 17 , wherein the phosphorus sulfide further satisfies formula (4):
25≤100× C/B≤ 60 (4)
wherein in the formula, C is peak areas of peaks that appear in a range of 56.6 ppm or more and 57.1 ppm or less in 31 PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31 PNMR spectroscopy.