System and method of producing thin-film electrolyte

• US 6,852,139 B2
• Filed: 07/11/2003
• Issued: 02/08/2005
• Est. Priority Date: 07/11/2003
• Status: Active Grant

• Current Assignee: Johnson Ip Holding Llc
• Original Assignee: Excellatron Solid State, LLC
• Inventors: Zhang, Ji-Guang, Maxie, Eleston, Meda, Lamartine
• Primary Examiner(s): Maples, John S.
• Application Number:
  US10/617,839
• Publication Number:
  US 20050008772A1
• Time in Patent Office: 578 Days
• Field of Search: 296/235, 429/322, 429/162, 423/306
• US Class Current: 29/623.5
• CPC Class Codes: C23C 16/30 Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
• CPC Class Codes: C23C 16/513 using plasma jets
• CPC Class Codes: H01M 10/052 Li-accumulators
• CPC Class Codes: H01M 10/0562 Solid materials
• CPC Class Codes: Y02E 60/10 Energy storage using batteries
• CPC Class Codes: Y02P 70/50 Manufacturing or production processes characterised by the final manufactured product
• CPC Class Codes: Y10T 29/49115 including coating or impregnating

Abstract

A process of producing a thin film electrolyte is provided wherein a volatile lithium-containing precursor and a volatile phosphate-containing precursor are mixed into a plasma generated from a plasma source. The mixture is then deposited upon a substrate. The process is conducted with the use of a system (11) having a plasma source (13) having a primary plenum (16) and a secondary plenum (23). The primary plenum is in fluid communication with a source of nitrogen gas (47) and a source of hydrogen gas (51). The secondary plenum is in fluid communication with a first bubbler (31) and a second bubbler (38).

Claims

1. A process for producing a solid electrolyte thin film comprising the steps of:

(a) providing a plasma source coupled to a supply of plasma gas so as to emit a plasma stream that is directed to a substrate positioned adjacent the plasma source;

(b) vaporizing a volatile lithium containing precursor;

(c) vaporizing a volatile phosphate containing precursor;

(d) transporting the vaporized volatile lithium containing precursor to the plasma source;

(e) transporting the vaporized volatile phosphate containing precursor to the plasma source; and

(f) expelling the vaporized volatile lithium containing precursor and vaporized volatile phosphate containing precursor from the plasma source and into the plasma stream emitted from the plasma source,

whereby the volatile lithium containing precursor and volatile phosphate containing precursor are prevented from mixing with the plasma gas prior to the gas being expelled from the plasma source as a plasma stream.

2. The process of claim 1 wherein the volatile lithium containing precursor is selected from the group consisting of lithium tert-butoxide, lithium hexafluroisoproxide, and lithium tetramethylheptane dionate.

3. The process of claim 1 wherein the volatile phosphate containing precursor is selected from the group consisting of triethylphosphate and trimethyl phosphate.

4. The process of claim 3 wherein the volatile lithium containing precursor is selected from the group consisting of lithium tert-butoxide, lithium hexafluoroisoproxide, and lithium tetramethylheptanedionate.

5. The process of claim 1 wherein the plasma gas is non-reactive with the volatile lithium-containing precursor.

6. The process of claim 1 wherein the plasma gas is reactive with the volatile lithium containing precursor.

7. The process of claim 6 wherein the plasma gas is selected from the group consisting of hydrogen and oxygen.

8. The process of claim 1 wherein the volatile lithium containing precursor is vaporized in step (b) with a metal organic bubbler.

9. The process of claim 1 wherein the volatile phosphate containing precursor is vaporized in step (c) with a metal organic bubbler.

10. A process for producing a thin film electrolyte layer comprising the steps of:

(a) generating a plasma from a plasma gas;

(b) vaporizing a volatile lithium containing precursor;

(c) vaporizing a volatile phosphate containing precursor;

(d) directing the vaporized volatile lithium containing precursor into the generated plasma;

(e) directing the vaporized volatile phosphate containing precursor into the generated plasma; and

(f) directing the plasma mixed with the volatile lithium containing precursor and the volatile phosphate containing precursor onto a substrate,

whereby the volatile lithium containing precursor and volatile phosphate containing precursor are mixed into the plasma gas only after the plasma is generated.

11. The process of claim 10 wherein the volatile lithium containing precursor is selected from the group consisting of lithium tert-butoxide, lithium hexafluoroisoproxide, and lithium tetramethylheptanedionate.

12. The process of claim 10 wherein the volatile phosphate containing precursor is selected from the group consisting of triethylphosphate and trimethyl phosphate.

13. The process of claim 12 wherein the volatile lithium containing precursor is selected from the group consisting of lithium tert-butoxide, lithium hexafluroisoproxide, and lithium tetramethylheptane dionate.

14. The process of claim 10 wherein the plasma gas is non-reactive with the volatile lithium containing precursor.

15. The process of claim 10 wherein the plasma gas is reactive with the volatile lithium containing precursor.

16. The process of claim 15 wherein the plasma gas is selected from the group consisting of hydrogen and oxygen.

17. The process of claim 10 wherein the volatile lithium containing precursor is vaporized in step (b) with a metal organic bubbler.

18. The process of claim 10 wherein the volatile phosphate containing precursor is vaporized in step (c) with a metal organic bubbler.