Method of making thin films of sodium fluorides and their derivatives by ALD

Patent metadata

Field	Value
Publication number	US-12065738-B2
Application number	US-202117508802-A
Country	US
Kind code	B2
Filing date	Oct 22, 2021
Priority date	Oct 22, 2021
Publication date	Aug 20, 2024
Grant date	Aug 20, 2024

Abstract

A method of making thin films of sodium fluorides and their derivatives by atomic layer deposition (“ALD”). A sodium precursor is exposed to a substrate in an ALD reactor. The sodium precursor is purged, leaving the substrate with a sodium intermediate bound thereon. A fluorine precursor is exposed to the bound sodium intermediate in the ALD reactor. The fluorine precursor is purged and a sodium fluoride film is formed on the substrate.

First claim

We claim:

1. A method for deposition of sodium fluoride comprising:
providing a substrate;
performing an atomic layer deposition having:
a first half reaction exposing a sodium precursor to the substrate at a first half reaction temperature, forming a sodium intermediate; and
a second half reaction exposing a fluorine precursor to the sodium intermediate; and

reacting the sodium intermediate with the fluorine precursor forming a sodium fluoride coating on the substrate.

2. The method of claim 1 , wherein the substrate is silicon, quartz, ALO, carbon nanotubes, cathodes, or silicon oxide.

3. The method of claim 1 , wherein the sodium precursor is tert-butoxide.

4. The method of claim 3 , wherein the sodium intermediate is Na(O t Bu) 1−x .

5. The method of claim 1 , wherein the fluorine precursor is selected from the group consisting of sulfur tetrafluoride, ammonium fluoride, WF 6 , and/or Hf-pyridine.

6. The method of claim 1 , wherein the first half reaction temperature is 175-250° C.

7. The method of claim 1 , further comprising a first purge step after the first half reaction exposure, the first purge step including exposure of a purge gas to the substrate and purging the sodium precursor.

8. The method of claim 1 , further comprising a second purge step after the second half reaction exposure, the second purge step including exposure of a purge gas to the substrate and purging the fluorine precursor.

9. A method for deposition of sodium fluoride comprising:
providing a substrate;
performing an atomic layer deposition having:
a first half reaction exposing a sodium precursor to the substrate at a first half reaction temperature, forming a sodium intermediate; and
a second half reaction exposing a Hf-pyridine precursor to the sodium intermediate; and

reacting the sodium intermediate with the Hf-pyridine precursor forming a sodium fluoride coating on the substrate.

10. The method of claim 9 , wherein the substrate is silicon, quartz, ALO, carbon nanotubes, cathodes, or silicon oxide.

11. The method of claim 9 , wherein the sodium precursor is tert-butoxide.

12. The method of claim 11 , wherein the sodium intermediate is Na(O t Bu) 1−x .

13. The method of claim 9 , further comprising a first purge step after the first half reaction exposure, the first purge step including exposure of a purge gas to the substrate and purging the sodium precursor.

14. The method of claim 9 , further comprising a second purge step after the second half reaction exposure, the second purge step including exposure of a purge gas to the substrate and purging the fluorine precursor.

15. A method for deposition of sodium fluoride comprising:
providing a substrate;
performing an atomic layer deposition having:
a first half reaction exposing a sodium precursor to the substrate at a first half reaction temperature, forming a sodium intermediate; and
a second half reaction exposing a WF 6 precursor to the sodium intermediate; and

reacting the sodium intermediate with the WF 6 precursor forming a sodium fluoride coating on the substrate.

16. The method of claim 15 , wherein the substrate is silicon, quartz, ALO, carbon nanotubes, cathodes, or silicon oxide.

17. The method of claim 15 , wherein the sodium precursor is tert-butoxide.

18. The method of claim 17 , wherein the sodium intermediate is Na(O t Bu) 1−x .

19. The method of claim 15 , further comprising a first purge step after the first half reaction exposure, the first purge step including exposure of a purge gas to the substrate and purging the sodium precursor.

20. The method of claim 15 , further comprising a second purge step after the second half reaction exposure, the second purge step including exposure of a purge gas to the substrate and purging the fluorine precursor.

Assignees

• Uchicago Argonne Llc
• Univ Boise State

Inventors

• Mane Anil U
• Elam Jeffrey W
• Kang Donghyeon
• Kuraitis Sara
• Graugnard Elton

Classifications

• C23C16/45527

  characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations · CPC title

• C23C16/52

  Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)} · CPC title

• C23C16/4408

  by purging residual gases from the reaction chamber or gas lines · CPC title

• C23C16/45553 Primary

  characterized by the use of precursors specially adapted for ALD · CPC title

• Y02E60/10

  Energy storage using batteries · CPC title