Method for purification and storage of Til4 for Ti-containing film deposition

Patent metadata

Field	Value
Publication number	US-10287175-B1
Application number	US-201514983780-A
Country	US
Kind code	B1
Filing date	Dec 30, 2015
Priority date	Dec 30, 2015
Publication date	May 14, 2019
Grant date	May 14, 2019

Abstract

Disclosed are methods for purification of a crude TiI4 for deposition of Ti-containing films including evaporating volatile impurities in the crude TiI4 under vacuum at room temperature in a sublimator and removing the volatile impurities, placing the sublimator in a hot oil bath under vacuum at a temperature to evaporate TiI4 and form powders or a solid, and sublimating the powers or the solid under vacuum at the temperature to obtain the purified TiI4. Disclosed are methods for storage of a pure TiI4 including drying a stainless-steel canister, instantaneously moving the dried stainless steel canister into a glove box under inert atmosphere at room temperature, moving the pure TiI4 into the glove box, filling the pure TiI4 into the dried stainless-steel canister, and sealing the dried stainless steel canister containing the pure TiI4 with metallic sealing.

First claim

We claim:

1. A method for purification of TiI 4 for deposition of Ti-containing films, the method comprising the steps of:
introducing TiI 4 into a sublimator having a cold trap cooled by liquid nitrogen;
evaporating volatile impurities in the TiI 4 under vacuum at room temperature to produce semi-purified TiI 4 and collecting the evaporated volatile impurities in the cold trap;
removing the evaporated volatile impurities from the cold trap;
placing the sublimator containing the semi-purified TiI 4 in a hot oil bath under vacuum at a temperature to evaporate TiI 4 and form a powder or solid in the cold trap; and
sublimating the powder or solid under vacuum at the temperature to obtain the purified TiI 4 .

2. The method of claim 1 , wherein the crude TiI 4 has a purity ranging from approximately 90% w/w to approximately 95% w/w.

3. The method of claim 1 , wherein the temperature ranges from approximately 150° C. to approximately 190° C.

4. The method of claim 3 , wherein the temperature is 180° C.

5. The method of any claim of 1 , wherein the volatile impurity is I 2 .

6. The method of any claim of 1 , wherein the volatile impurity is HI.

7. The method of claim 1 , wherein the purified TiI 4 has a purity of 99% w/w.

8. The method of claim 1 , wherein the purified TiI 4 has a purity ranging from approximately 99% w/w to approximately 100% w/w.

9. The method of claim 1 , wherein the purified TiI 4 has a purity ranging from approximately 99.9% w/w to approximately 100.0% w/w.

10. The method of claim 1 , wherein the purified TiI 4 contains between 0% w/w and approximately 1% w/w non-volatile impurities.

11. The method of claim 1 , wherein the purified TiI 4 contains between 0% w/w and approximately 0.5% w/w non-volatile impurities.

12. The method of claim 1 , wherein the purified TiI 4 contains between 0% w/w and approximately 1% w/w I 2 and/or HI.

13. The method of claim 1 , wherein the purified TiI 4 contains between 0% w/w and approximately 0.5% w/w I 2 and/or HI.

Assignees

• Air Liquide

Inventors

• Gatineau Satoko
• Nikiforov Grigory

Classifications

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title

• C01G23/02 Primary

  Halides of titanium · CPC title

• C01P2006/80

  Compositional purity · CPC title

• B65B7/16

  Closing semi-rigid or rigid containers or receptacles not deformed by, or not taking-up shape of, contents, e.g. boxes or cartons · CPC title

• B65B31/00

  Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers · CPC title