Sustained self-sputtering of lithium for lithium physical vapor deposition

• US 10,443,121 B2
• Filed: 04/24/2014
• Issued: 10/15/2019
• Est. Priority Date: 04/24/2013
• Status: Active Grant

• Current Assignee: View Incorporated
• Original Assignee: View Incorporated
• Inventors: Neumann, Martin John
• Primary Examiner(s): Brayton, John J
• Application Number:
  US14/784,276
• Publication Number:
  US 20160076139A1
• Time in Patent Office: 2,000 Days
• CPC Class Codes: C23C 14/185 by cathodic sputtering
• CPC Class Codes: C23C 14/3457 using other particles than noble gas ions C23C14/0036, C23C14/46 take precedence
• CPC Class Codes: C23C 14/3492 Variation of parameters during sputtering
• CPC Class Codes: C23C 14/54 Controlling or regulating the coating process
• CPC Class Codes: H01J 2237/036 Spacing
• CPC Class Codes: H01J 2237/202 Movement
• CPC Class Codes: H01J 2237/2487 using digital signal processors
• CPC Class Codes: H01J 2237/327 Arrangements for generating the plasma
• CPC Class Codes: H01J 2237/332 Coating
• CPC Class Codes: H01J 37/32733 Means for moving the material to be treated
• CPC Class Codes: H01J 37/3426 Material
• CPC Class Codes: H01J 37/3476 Testing and control

Abstract

A method of sustained self-sputtering of lithium in a sputtering station having a lithium metal target, the method comprising initiating a lithium sputtering reaction in the sputtering station by igniting an initial plasma comprising a majority fraction of inert gas ions and inducing a sustained lithium self-sputtering reaction by reducing supply of an inert gas to the sputtering station under conditions that provide a sustained self-sputtering lithium plasma comprising a majority fraction of lithium ions.

Claims

1. A method of sustained self-sputtering of lithium in a sputtering station having a lithium metal target in a chamber, the method comprising:

flowing an inert gas to the chamber;

initiating a lithium sputtering reaction in the sputtering station by igniting an initial plasma comprising a majority fraction of inert gas ions; and

inducing a sustained lithium self-sputtering reaction by reducing the flow of the inert gas to the sputtering station under conditions that provide a sustained self-sputtering lithium plasma comprising a majority fraction of lithium ions having a mean free path of between 6.1 cm and 61 cm, wherein the conditions include applying a voltage between an anode and the lithium metal target that is a cathode that is between 200 V and 500 V.

2. The method of claim 1, further comprising incorporating lithium from the lithium metal target into a workpiece while the workpiece is in the sputtering station, wherein the workpiece comprises a partially fabricated electrochromic device.

3. The method of claim 2, wherein the lithium is incorporated into one or more layers of the partially fabricated electrochromic device.

4. The method of claim 3, wherein one of the one or more layers of the partially fabricated electrochromic device is an anodically coloring electrochromic material layer comprising one of nickel, tungsten, and oxygen.

5. The method of claim 1, wherein the conditions that provide the sustained self-sputtering lithium plasma include one or more of maintaining a mean free path of lithium ions below a predefined level and maintaining a sputter yield above 1.0.

6. The method of claim 1, further comprising maintaining the sustained self-sputtering lithium plasma by adjusting process parameters.

7. The method of claim 6, wherein adjusting process parameters comprises one or more of:

maintaining power to a cathode of the sputtering station above a pre-defined level;

maintaining absolute pressure in the sputtering station between 0.1 and 1.0 mT; and

maintaining a mean free path of lithium ions to below a pre-defined level.

8. The method of claim 1, further comprising adjusting lithium flux to within a predefined range based on measurements from a sensor.

9. The method of claim 8, wherein the lithium flux is adjusted by moving a workpiece relative to the lithium metal target.

10. A sustained lithium self-sputtering apparatus comprising:

a sputtering station comprising;

a chamber;

an anode in the chamber;

a lithium metal target in the chamber, wherein the lithium metal target is a cathode;

a voltage source electrically connected to the anode and to the cathode; and

an inlet that regulates flow of an inert gas to the chamber during operation; and

a controller containing program instructions for;

controlling conditions in the sputtering station to induce and maintain a sustained self-sputtering lithium plasma in which lithium ions have a mean free path of between 6.1 cm and 61 cm,

controlling the inlet to regulate the flow of inert gas to the chamber during operation, including flowing the inert gas to the chamber and reducing the flow of the inert gas after the sustained self-sputtering lithium plasma is induced without extinguishing the sustained self-sputtering lithium plasma, and

controlling the voltage source to coordinate delivery of a potential between the anode and the cathode that is between 200 V and 500 V.

11. The sustained lithium self-sputtering apparatus of claim 10, wherein the anode is a part of a wall of the chamber.

12. The sustained lithium self-sputtering apparatus of claim 10, wherein the lithium metal target is made of at least 75% lithium metal.

13. The sustained lithium self-sputtering apparatus of claim 10, wherein lithium sputtered from the lithium metal target in the presence of the sustained self-sputtering lithium plasma is incorporated into a workpiece while the workpiece is present in the chamber of the sputtering station.

14. The sustained lithium self-sputtering apparatus of claim 13, wherein the workpiece is located within a predefined distance from the cathode, and wherein the workpiece comprises a partially fabricated electrochromic device.

15. The sustained lithium self-sputtering apparatus of claim 14, wherein one of the one or more layers of the partially fabricated electrochromic device is an anodically coloring electrochromic material layer comprising one of nickel, tungsten, and oxygen.

16. The sustained lithium self-sputtering apparatus of claim 10, wherein the controller contains further program instructions for maintaining absolute pressure in the sputtering station between 0.1 and 1.0 mT.

17. The sustained lithium self-sputtering apparatus of claim 10, wherein the controller contains further program instructions for maintaining a sputter yield of greater than one, wherein the sputter yield is the number of lithium atoms ejected from the lithium metal target per incident lithium atom.

18. The sustained lithium self-sputtering apparatus of claim 10, wherein the controller contains further program instructions for communicating signals to the voltage source to increase power to the cathode to above a predefined level.

19. The sustained lithium self-sputtering apparatus of claim 10, further comprising a sensor in communication with the controller, wherein the controller contains further program instructions for adjusting lithium flux to the workpiece based on measurements from the sensor.

20. The sustained lithium self-sputtering apparatus of claim 19, further comprising a mechanism for moving the workpiece relative to the lithium metal target, the mechanism in communication with the controller, wherein the lithium flux is adjusted by sending signals to the mechanism to move the workpiece relative to the lithium metal target.

21. The sustained lithium self-sputtering apparatus of claim 10, wherein the distance between the anode and the cathode is greater than 100 cm.

22. The sustained lithium self-sputtering apparatus of claim 10, wherein the distance between the anode and the cathode is between 60 cm and 100 cm.

23. The sustained lithium self-sputtering apparatus of claim 10, wherein the controller contains further program instructions for controlling conditions in the sputtering station such that the sustained self-sputtering lithium plasma includes one or both a mean free path of lithium ions below a predefined level and a sputter yield above 1.0, wherein the sputter yield is the number of lithium atoms ejected from the lithium metal target per incident lithium ion.

24. The sustained lithium self-sputtering apparatus of claim 10, wherein the inert gas is helium.

25. The sustained lithium self-sputtering apparatus of claim 10, wherein the distance between the anode and the cathode is greater than the mean free path of the sustained self-sputtering lithium plasma.