1. A choline salt of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol.
2. A choline salt crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having an endothermic peak at 194 to 198\xb0 C. measured by differential scanning calorimetry (DSC analysis).
3. A choline salt crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having main peaks at about 2\u03b8 (\xb0) of 5.58, 14.72, 16.80, 17.82, 21.02, and 22.46 measured by X-ray powder diffraction.
4. A choline salt crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having an endothermic peak at 194 to 198\xb0 C. measured by differential scanning calorimetry (DSC analysis) and main peaks at about 2\u03b8 (\xb0) of 5.58, 14.72, 16.80, 17.82, 21.02, and 22.46 measured by X-ray powder diffraction.
5. A choline salt hydrate crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having a broad endothermic peak at about 78\xb0 C. and an endothermic peak at 195 to 199\xb0 C. measured by differential scanning calorimetry (DSC analysis).
6. A choline salt hydrate crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having main peaks at about 2\u03b8 (\xb0) of 5.66, 17.08, 17.66, 19.02, 19.58, and 22.14 measured by X-ray powder diffraction.
7. A choline salt hydrate crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having a broad endothermic peak at about 78\xb0 C. and an endothermic peak at 195 to 199\xb0 C. measured by differential scanning calorimetry (DSC analysis) and main peaks at about 2\u03b8 (\xb0) of 5.66, 17.08, 17.66, 19.02, 19.58, and 22.14 measured by X-ray powder diffraction.
8. (canceled)
9. (canceled)
10. (canceled)
11. A pharmaceutical composition comprising the choline salt crystal selected from the group consisting of a choline salt of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol, a choline salt crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having an endothermic peak at 194 to 198\xb0 C. measured by differential scanning calorimetry (DSC analysis), a choline salt crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having main peaks at about 2\u03b8 (\xb0) of 5.58, 14.72, 16.80, 17.82, 21.02, and 22.46 measured by X-ray powder diffraction, a choline salt crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having an endothermic peak at 194 to 198\xb0 C. measured by differential scanning calorimetry (DSC analysis) and main peaks at about 2\u03b8 (\xb0) of 5.58, 14.72, 16.80, 17.82, 21.02, and 22.46 measured by X-ray powder diffraction, a choline salt hydrate crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having a broad endothermic peak at about 78\xb0 C. and an endothermic peak at 195 to 199\xb0 C. measured by differential scanning calorimetry (DSC analysis), a choline salt hydrate crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having main peaks at about 2\u03b8 (\xb0) of 5.66, 17.08, 17.66, 19.02, 19.58, and 22.14 measured by X-ray powder diffraction, and a choline salt hydrate crystal of (1S)-1,5-anhydro-1-5-(azulen-2-ylmethyl)-2-hydroxyphenyl-D-glucitol having a broad endothermic peak at about 78\xb0 C. and an endothermic peak at 195 to 199\xb0 C. measured by differential scanning calorimetry (DSC analysis) and main peaks at about 2\u03b8 (\xb0) of 5.66, 17.08, 17.66, 19.02, 19.58, and 22.14 measured by X-ray powder diffraction as an effective ingredient.
12. The pharmaceutical composition according to claim 11, further comprising a pharmaceutically acceptable excipient.
13. The pharmaceutical composition according to claim 11, which is a diabetes treating agent.
14. The pharmaceutical composition according to claim 12, which is a diabetes treating agent.
The claims below are in addition to those above.
All refrences to claim(s) which appear below refer to the numbering after this setence.
We claim as our invention:
1. A semiconductor device, comprising:
(a) a silicon nitride film disposed along the surface of a dielectric material within a recess formed in the dielectric material; and,
(b) a refractory metal film overlaying the silicon nitride film.
2. The semiconductor device of claim 1 in which the silicon nitride film is formed from a process in which the dielectric material comprises silicon and is exposed to a nitrogen-containing material converting the chemical composition of at least a portion of the dielectric material adjacent to the recess to silicon nitride.
3. The semiconductor device of claim 2 in which the dielectric material is exposed to the nitrogen source at a predetermined temperature and pressure, for a timed duration.
4. The semiconductor device of claim 1 wherein said semiconductor device further includes an etch stop layer overlaying the dielectric material and said recess is formed in the etch stop layer and the dielectric material, and said sidewalls of the recess include a surface of the etch stop layer, and said silicon nitride film is disposed along the surface of the dielectric material within the recess, but not along the surface of the etch stop layer within the recess.
5. The semiconductor device of claim 1 wherein said recess sidewalls include a plurality of surfaces of dielectric material spaced apart within the recess and the silicon nitride film is disposed along each said surface of the dielectric material.
6. The semiconductor device of claim 4 wherein said refractory metal film is conformally deposited within the recess, over the silicon nitride film and surfaces of the etch stop layer.
7. The semiconductor device of claim 1 wherein said recess is a trench formed in the dielectric material.
8. The semiconductor device of claim 1 wherein said feature includes a via and a trench formed in the dielectric material.
9. The semiconductor device of claim 1 wherein said recess includes a via formed in the dielectric material.
10. A semiconductor device, comprising:
(a) two metal layers separated by an insulating layer;
(b) a recess formed in the two metal layers and insulating layer, and exposing a surface of at least one dielectric material within the recess;
(c) a conductive metal deposited within, and filling said recess;
(d) a barrier layer formed in the recess between the dielectric material and the conductive metal, having a silicon nitride film disposed along the surface of the dielectric material and a refractory metal layer between the silicon nitride film and the conductive metal; and,
(e) said refractory metal layer interposed between the copper in the recess in one of the metal layers and the insulating layer.
11. The semiconductor device of claim 10 wherein said at least one dielectric material comprises a low-k dielectric material.
12. The semiconductor device of claim 10 further comprising two etch stop layers, and each etch stop layer is interposed between the insulating layer and a respective metal layer, and said recess having a plurality of surfaces of the dielectric material therein spaced apart by a surface of the etch stop layer, and said silicon nitride film is disposed along the surface of the dielectric material, but not along etch stop layer surface.
13. The semiconductor of claim 10 wherein in said recess comprises a trench formed in each of the two metal layers, and a via formed in the insulating layer interconnecting the trenches of the metal layers.
14. A process for the fabrication of a semiconductor device, comprising the steps of:
(a) forming a silicon nitride film within a recess formed within a dielectric material; and,
(b) forming a refractory metal film over the silicon nitride films within the recess formed in the dielectric material.
15. The process of claim 14 wherein said step of forming the silicon nitride film comprises converting the chemical composition of at least a portion of the dielectric material adjacent to the recess to silicon nitride by exposing the surface of the dielectric material to a nitrogen-containing material.
16. The process of claim 15 wherein the dielectric material is exposed to the nitrogen-containing material at a predetermined temperature and pressure, for a timed duration.
17. The process of claim 14 wherein said step of converting the chemical composition of the dielectric material comprises providing a deposition chamber in which the semiconductor device is fixed, generating a plasma within the reaction chamber adjacent to the semiconductor device and injecting nitrogen into the reaction chamber and plasma.
18. The process of claim 15 wherein the step of converting the chemical composition of the dielectric material further comprises elevating a temperature within the reaction chamber within the range of about 250 C. to about 270, maintaining the pressure within the chamber within the range of about 400 mtorr to about 1000 mtorr, and maintaining said temperature and pressure for about 120 seconds.
19. The process of claim 14 further comprising the step of forming at least one etch stop layer on the semiconductor adjacent the dielectric layer and said step of forming the recess includes forming the recess in said etch stop layer and dielectric layer whereby the sidewall of the recess includes a surface of the etch stop layer and the surface of the dielectric material.
20. The process of claim 19 wherein the step of forming a silicon nitride film comprises forming said silicon nitride film along the surface of the dielectric material within the recess, and not along the surface of the etch stop layer within the recess.
21. The process of claim 21 wherein the step of forming the refractory metal film includes depositing the refractory metal film over the silicon nitride film and the surface of the etch stop layer.