Plasma resistant multi-layer architecture for high aspect ratio parts

Patent metadata

Field	Value
Publication number	US-10858741-B2
Application number	US-201916298964-A
Country	US
Kind code	B2
Filing date	Mar 11, 2019
Priority date	Mar 11, 2019
Publication date	Dec 8, 2020
Grant date	Dec 8, 2020

Abstract

Disclosed herein is an article comprising one or more channels and a multi-layer protective coating on the one or more channels. The multi-layer protective coating includes an anodization layer comprising a plurality of cracks and a plurality of pores, a sealing layer on the anodization layer, and a top layer on the sealing layer. The sealing layer comprises a metal oxide, the seals the plurality of cracks and the plurality of pores, and has a porosity of approximately 0%. The top layer comprises a rare earth oxide, a rare earth fluoride, or a rare earth oxyfluoride, has a different material composition than the sealing layer, and has a porosity of approximately 0%.

First claim

What is claimed is:

1. An article comprising:
one or more channels; and
a multi-layer protective coating on the one or more channels, the multi-layer protective coating comprising:
an anodization layer, the anodization layer comprising a plurality of cracks and a plurality of pores;
a sealing layer on the anodization layer, wherein the sealing layer comprises a metal oxide, and wherein the sealing layer seals the plurality of cracks and the plurality of pores, the sealing layer having a porosity of approximately 0%; and
a top layer on the sealing layer, wherein the top layer comprises a metal oxide, a rare earth oxide, a rare earth fluoride, or a rare earth oxyfluoride, wherein the top layer has a same or a different material composition as compared to the sealing layer, and wherein the top layer has a porosity of approximately 0%;

wherein the multi-layer protective coating has a dielectric breakdown voltage of at least 2000 Volts.

2. The article of claim 1 , wherein the one or more channels comprise a length to diameter aspect ratio of greater than about 5:1.

3. The article of claim 1 , wherein the sealing layer consists essentially of Al 2 O 3 .

4. The article of claim 1 , wherein:
a thickness of the anodization layer is about 100 nm to about 90 microns; and
a combined thickness of the sealing layer and the top layer is about 1-5 microns.

5. The article of claim 1 , wherein the top layer comprises the metal oxide or the rare earth oxide, and wherein the rare earth oxide is selected from a group consisting of Y 2 O 3 , Al 2 O 3 , Y 3 Al 5 O 12 (YAG), Y 4 Al 2 O 9 (YAM), YAlO 3 (YAP), Er 2 O 3 , Er 3 Al 5 O 12 (EAG), ZrO 2 , Gd 2 O 3 , a solid solution of Y 2 O 3 —ZrO 2 , and a ceramic compound comprising Y 4 Al 2 O 9 and a solid-solution of Y 2 O 3 —ZrO 2 .

6. The article of claim 1 , wherein the top layer comprises the rare earth fluoride, and wherein the rare earth fluoride is selected from a group consisting of YF 3 , ErF 3 , ZrF 4 and GdF 3 .

7. The article of claim 1 , wherein the top layer comprises the rare earth oxyfluoride, and wherein the rare earth oxyfluoride is selected from a group consisting of yttrium oxyfluoride, erbium oxyfluoride, zirconium oxyfluoride, aluminum oxyfluoride, and gadolinium oxyfluoride.

8. The article of claim 1 , wherein the sealing layer is selected from a group consisting of Y 2 O 3 , Y 3 Al 5 O 12 (YAG), Y 4 Al 2 O 9 (YAM), YAlO 3 (YAP), Er 2 O 3 , Er 3 Al 5 O 12 (EAG), ZrO 2 , Gd 2 O 3 , a solid solution of Y 2 O 3 —ZrO 2 , Al 2 O 3 , and a ceramic compound comprising Y 4 Al 2 O 9 and a solid-solution of Y 2 O 3 —ZrO 2 .

9. The article of claim 1 , wherein the article comprises aluminum or an aluminum alloy, and wherein the article comprises a remote plasma delivery cylinder.

10. The article of claim 1 , wherein an electrical impedance of the multi-layer protective coating has approximately a same electrical impedance before exposure to a temperature of between about 120° C. and about 350° C. and after exposure to the temperature of between about 120° C. and about 350° C.

11. A plurality of articles, wherein:
each article of the plurality of articles comprises:
one or more channels; and
a multi-layer protective coating on the one or more channels, the multi-layer protective coating comprising:
an anodization layer, the anodization layer comprising a plurality of cracks and a plurality of pores;
a sealing layer on the anodization layer, wherein the sealing layer comprises Al 2 O 3 , and wherein the sealing layer seals the plurality of cracks and the plurality of pores, the sealing layer having a porosity of approximately 0%; and
a top layer on the sealing layer, wherein the top layer comprises a metal oxide, a rare earth oxide, a rare earth fluoride, or a rare earth oxyfluoride, wherein the top layer has a same or a different material composition as compared to the sealing layer, and wherein the top layer has a porosity of approximately 0%;

wherein a part to part variation of a dielectric breakdown voltage between the plurality of articles, as measured at the one or more channels of the plurality of articles, is less than about +/−5%.

12. The plurality of articles of claim 11 , wherein the dielectric breakdown voltage of the one or more channels for each of the plurality of articles is over 2000 Volts.

13. A method of forming a multi-layer protective coating on one or more channels of one or more articles, comprising:
anodizing a surface of the one or more channels of a first article to form an anodization layer on the one or more channels, the anodization layer comprising a plurality of cracks and a plurality of pores;
depositing a sealing layer onto the anodization layer using an atomic layer deposition (ALD) process, wherein the sealing layer comprises a metal oxide, and wherein the sealing layer seals the plurality of cracks and the plurality of pores, the sealing layer having a porosity of approximately 0%; and
depositing a top layer onto the sealing layer using the ALD process, wherein the top layer comprises a metal oxide, a rare earth oxide, a rare earth fluoride, or a rare earth oxyfluoride, wherein the top layer has a same or a different material composition as compared to the sealing layer, and wherein the top layer has a porosity of approximately 0%;
wherein the multi-layer protective coating has a dielectric breakdown voltage of at least 2000 Volts.

14. The method of claim 13 , wherein the sealing layer consists essentially of Al 2 O 3 .

15. The method of claim 13 , wherein the anodization layer has a thickness of about 0.5 microns to about 90 microns and a combined thickness of the sealing layer and the top layer is about 1-5 microns.

16. The method of claim 13 , further comprising:
anodizing surfaces of the one or more channels of a plurality of additional articles to form an anodization layer on the one or more channels of the plurality of additional articles;
depositing a sealing layer onto the anodization layer of the plurality of additional articles using the ALD process; and
depositing a top layer onto the sealing layer of the plurality of additional articles using the ALD process;
wherein a part to part variation of the dielectric breakdown voltage between the first article and the plurality of additional articles is less than about +/−5%.

17. The method of claim 13 , wherein the top layer comprises the rare earth oxide, wherein the rare earth oxide comprises a mixture of at least a first metal and a second metal, and wherein depositing the top layer comprises:
performing a deposition cycle comprising:
injecting a first precursor for the first metal into a deposition chamber containing the first article to cause the first precursor to adsorb onto a surface of the one or more channels;
subsequently injecting a second precursor for the second metal into the deposition chamber containing the first article to cause the second precursor to adsorb onto the surface of the one or more channels; and
subsequently injecting an oxygen-containing reactant into the deposition chamber; and

repeating the deposition cycle one or more times until a target thickness is reached for the top layer.

18. The method of claim 13 , wherein the top layer comprises the rare earth oxyfluoride, and wherein depositing the top layer comprises:
performing a deposition cycle comprising:
injecting a first precursor for a rare earth metal into a deposition chamber containing the first article to cause the first precursor to adsorb onto a surface of the one or more channels;
subsequen

Assignees

• Applied Materials Inc

Inventors

• He Xiao-Ming
• Sun Jennifer Y

Classifications

• H01J37/32495

  Means for protecting the vessel against plasma · CPC title

• 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

• C23C16/452

  by activating reactive gas streams before {their} introduction into the reaction chamber, e.g. by {ionisation} or addition of reactive species · CPC title

• C23C16/4404

  Coatings or surface treatment on the inside of the reaction chamber or on parts thereof · CPC title

• C23C16/40

  Oxides · CPC title