SiO2 thin film produced by atomic layer deposition at room temperature

Patent metadata

Field	Value
Publication number	US-11041238-B2
Application number	US-201615751389-A
Country	US
Kind code	B2
Filing date	Aug 8, 2016
Priority date	Aug 10, 2015
Publication date	Jun 22, 2021
Grant date	Jun 22, 2021

Abstract

A process of atomic layer deposition for the deposition of silicon oxide on a substrate, performed at room temperature, involving at least three precursors, being silicon tetrachloride, water and one Lewis base agent, being in various instances ammonia. The process comprises the steps of exposing on the substrate during an exposure time (a) the one Lewis base agent, (b) the silicon tetrachloride, and (c) the water. The process is remarkable in that at least one step of purge with nitrogen gas is performed after each of the steps (a), (b) and (c) during a purge time. Additionally, a film of silicon oxide which is remarkable in that it comprises a low level of chlorine contaminant and a significant degree of porosity with pores, the pores being in various instances micropores, mesopores or nanopores.

First claim

The invention claimed is:

1. A process of atomic layer deposition for a coating of silicon oxide on a substrate, such as on an inorganic material, and performed at room temperature, involving at least three precursors, the at least three precursors being silicon tetrachloride, water and one Lewis base agent, said method comprising the sequential and non-overlapping steps of:
a) exposing the one Lewis base agent to the substrate during a first exposure time;
b) exposing the silicon tetrachloride to the substrate during a second exposure time; and
c) exposing the water to the substrate during a third exposure time,
wherein a step of purging with nitrogen gas is performed after step (a), and at least one step of purging with nitrogen gas is performed after each of the steps (b) and (c),
wherein the at least one step of purging with nitrogen gas after each of steps (b) and (c) presents a ratio of nitrogen gas flow pressure which is inferior to one of 5 Torr, 4 Torr, 3 Torr, 2 Torr or 1 Torr,
thereby obtaining a porous silicon dioxide film onto said substrate, wherein the level of chlorine contaminants is less than 3% of the total mass of said silicon dioxide.

2. The process according to claim 1 , wherein the one Lewis base agent is ammonia.

3. The process according to claim 1 , wherein the at least one step of purge with nitrogen gas presents a ratio of nitrogen gas flow/total pressure inferior to 2 Torr.

4. The process according to claim 1 , wherein the exposure time of the precursors is comprised between 50 milliseconds and 200 seconds.

5. The process according to claim 1 , wherein
a) the exposure time of the silicon tetrachloride is comprised between 50 milliseconds and 200 milliseconds; and
b) the exposure time of the Lewis base agent and of the water is comprised between 1 second and 3 seconds.

6. The process according to claim 1 , wherein the exposure time of the precursors is comprised between 50 seconds and 200 seconds.

7. The process according to claim 1 , wherein the exposure time of the precursors is equal to 90 seconds.

8. The process according to claim 1 , wherein the purge time with nitrogen gas is comprised between 1 second and 20 seconds.

9. The process according to claim 1 , wherein
a) the purge time with nitrogen gas after step (a) is comprised between 100 seconds and 240 seconds;
b) the purge time with nitrogen gas after step (b) is comprised between 10 seconds and 100 seconds; and
c) the purge time with nitrogen gas after step (c) is comprised between 200 seconds and 360 seconds.

10. The process according to claim 1 , wherein the steps (a), (b) and (c) with concomitant purge steps are repeated between 50 and 5000 times.

11. The process according to claim 1 , wherein the substrate comprises an inorganic material that is composed of at least one of silicon, silicon oxide, titanium, titanium oxide, aluminium, aluminium oxide, zinc, zinc oxide, and any combinations thereof.

12. The process according to claim 1 , wherein the substrate comprises an inorganic material inorganic material composed of silicon.

13. The process according to claim 11 , wherein the silicon materials are cleaned using an RCA procedure before the steps of exposing.

14. The process according to claim 1 , wherein the process is carried out in a reactor that is equipped with a residual gas analyser adapted for determining the exposure time and the purge time.

15. The process according to claim 14 , wherein the reactor is further equipped with at least one of a quartz crystal microbalance adapted for the gravimetric monitoring of the film growth and a mass spectrometer adapted for monitoring the gas composition.

Assignees

• Luxembourg Inst Science & Tech List

Inventors

• Arl Didier
• Adjeroud Noureddine
• Lenoble Damien

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

• C23C16/45534 Primary

  Use of auxiliary reactants other than used for contributing to the composition of the main film, e.g. catalysts, activators or scavengers · CPC title

• C23C16/402

  Silicon dioxide · CPC title