High purity tungsten hexachloride and method for making same

Patent metadata

Field	Value
Publication number	US-2016305020-A1
Application number	US-201615096872-A
Country	US
Kind code	A1
Filing date	Apr 12, 2016
Priority date	Apr 17, 2015
Publication date	Oct 20, 2016
Grant date	—

Abstract

Condensable metal halide materials, such as but not limited to tungsten chloride (WCl 6 ), can be used deposit films metal or metal containing films in a chemical vapor deposition (CVD) or atomic layer deposition process. Described herein are high purity compositions comprising condensable materials and methods to purify condensable materials. In one aspect, there is provided a composition comprising: tungsten hexachloride which is substantially free of at least one impurity and wherein the tungsten hexachloride comprises at least 90%, preferably 95% and more preferably 99% by weight or greater of a β-WCl 6 and 5% by weight or less of the α-WCl 6 as measured by X-ray diffraction.

First claim

1 . A composition for depositing a tungsten film or tungsten-containing film by a chemical vapor deposition or atomic layer deposition process, the composition comprising:
at least 90% by weight or greater of β-WCl 6 .

2 . The composition of claim 1 , wherein the composition comprises at least 95% by weight or greater of β-WCl 6 and 5% by weight or less of α-WCl 6 .

3 . The composition of claim 2 , wherein the composition further comprises 1% by weight or less of WOCl 4 .

4 . The composition of claim 1 , wherein the composition comprises at least 99% by weight or greater of β-WCl 6 and 1% by weight or less of α-WCl 6 .

5 . The composition of claim 4 , wherein the composition comprises at least 99.9% by weight or greater of β-WCl 6 .

6 . A delivery system for depositing a tungsten film or tungsten-containing film comprising:
a composition comprising at least 90% by weight or greater of β-WCl 6 ; a vessel; and wherein the composition is inside the vessel.

7 . The delivery system of claim 6 , wherein the composition comprises at least 95% by weight or greater of β-WCl 6 and 5% by weight or less of α-WCl 6 .

8 . The delivery system of claim 6 , wherein the composition comprises at least 99.9% by weight or greater of β-WCl 6 and 1% by weight or less of α-WCl 6 .

9 . The delivery system of claim 6 , wherein the composition comprises at least 99.9% by weight or greater of β-WCl 6 .

10 . A process of preparing a delivery system for depositing a tungsten film or tungsten-containing film comprising:
providing a vessel; providing a composition comprising at least 90% by weight of WCl 6 wherein the composition is inside the vessel; and heating the vessel until 90.0% by weight of WCl 6 is β-WCl 6 .

11 . The process of claim 10 , wherein the heating is performed until 95.0% by weight of WCl 6 is β-WCl 6 .

12 . The process of claim 10 , wherein the heating is performed until 99.0% by weight of WCl 6 is β-WCl 6 .

13 . The process of claim 10 , wherein the heating is performed until 99.9% by weight of WCl 6 is β-WCl 6 .

14 . A system for purifying a crude material comprising WCl 6 and at least one impurity comprising:
(a) at least one boiler; (b) a condenser; (c) a connector in fluid communication with the boiler and the condenser; (d) a carrier gas in fluid communication with the boiler; and (e) a fluidizing gas in fluid communication with the connector and the condenser; wherein
the at least one impurity comprising at least one of trace metals, tungsten oxytetrachloride (WOCl 4 ), and tungsten pentachloride (WCl 5 );
the at least one boiler is maintained at a temperature above the boiling point of WCl 6 to convert filled crude material to gaseous phase mixing with the carrier gas to obtain boiler vapor stream;
the connector is filled with the boiler vapor stream;
the condenser containing the fluidizing gas mixing with the boiler vapor stream to obtain a condenser vapor containing purified material comprising WCl 6 at the bottom of the condenser while the fluidizing gas carrying the at least one impurity to the top of the condenser;
the carrier gas and the fluidizing gas are not react with WCl 6 ; and
the fluidizing gas is cooler than the boiler vapor stream.

15 . The system of claim 14 , wherein the at least one boiler is maintained at >300° C.; and the condenser vapor is maintained at one or more temperatures ranging from about 100 to about 180° C.

16 . The system of claim 14 ; wherein a molar ration of the fluidizing gas and the boiler vapor stream is <200:1; and a molar ration of the carrier gas to the crude material in the boiler vapor stream is <10:1.

17 . The system of claim 14 ; wherein the condenser further comprises a dip tube in fluid communication with a vacuum pump to withdraw the purified material comprising WCl 6 from the bottom of the condenser.

18 . The system of claim 14 ; wherein the purified material comprising WCl 6 comprises at least 90% by weight or greater of β-WCl 6 .

19 . The system of claim 14 ; wherein the purified material comprising WCl 6 comprises at least 99% by weight or greater of β-WCl 6 .

20 . The system of claim 14 ; wherein the system further comprises a vessel in fluid communication with the dip tube for housing the purified material comprising WCl 6 wherein the purified material comprising WCl 6 comprises at least 90% or 99% by weight or greater of β-WCl 6 .

Assignees

• Air Prod & Chem

Inventors

• Wu Xiaoxi
• Ivanov Sergei Vladimirovich

Classifications

• C01P2006/80

  Compositional purity · CPC title

• C01G41/04 Primary

  Halides · CPC title

• C23C16/4402

  Reduction of impurities in the source gas · CPC title

• B01D3/322

  Reboiler specifications · CPC title

• B01D3/346

  the gas being used for removing vapours, e.g. transport gas · CPC title