Condensable metal halide materials, such as but not limited to tungsten hexachloride and tungsten pentachloride 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 tungsten hexachloride an
Condensable metal halide materials, such as but not limited to tungsten hexachloride and tungsten pentachloride 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 tungsten hexachloride and tungsten pentachloride systems and methods to purify tungsten hexachloride and tungsten pentachloride raw materials. There is provided a purified tungsten hexachloride and tungsten pentachloride containing less than 10 ppm, preferably less than 5 ppm, more preferably less than 1 ppm, and most preferably less than 0.5 ppm of iron and/or molybdenum; and less than 10 ppm, preferably less than 5 ppm of all other trace metals combined including but not limited to aluminum, potassium and sodium.
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1. A method of purifying a solid phase raw material comprising tungsten chloride and at least one impurity, comprising: (a) heating the solid phase raw material in a first vessel to within a first temperature range to produce a heated raw material;(b) contacting the heated raw material with a getter
1. A method of purifying a solid phase raw material comprising tungsten chloride and at least one impurity, comprising: (a) heating the solid phase raw material in a first vessel to within a first temperature range to produce a heated raw material;(b) contacting the heated raw material with a getter, which results in a reaction between the getter and a reactive portion of the at least one impurity to produce at least one complexed impurity and produces a first intermediate product comprising tungsten chloride, an unreactive portion of the at least one impurity, and the at least one complexed impurity, wherein the at least one complexed impurity has a sublimation point that is greater than a sublimation point of the tungsten chloride and the getter is selected from the group consisting of: potassium chloride, sodium chloride, rubidium chloride, cesium chloride, calcium chloride, magnesium chloride, barium chloride, and combinations thereof;(c) performing a separation process on the first intermediate product which results in at least a portion of the at least one complexed impurity being separated from the tungsten chloride and the unreactive portion of the at least one impurity to produce a second intermediate product, the separation process selected from the group consisting of: distillation and sublimation;(d) cooling the second intermediate product to within a second temperature range, which results in at least a portion of the unreactive portion of the at least one impurity being separated from the tungsten chloride to produce a product, wherein the product is enriched in tungsten chloride relative to the solid phase raw material and the second intermediate product;wherein steps (a) through (d) are performed within a first pressure range. 2. The method of claim 1, further comprising: (e) cooling the unreactive portion of the at least one impurity to a third temperature range, to produce a condensed light impurity. 3. The method of claim 1, further comprising: (g) recovering the product produced in step d and using it as the solid phase raw material in step a. 4. The method of claim 1, wherein step a comprises heating the solid phase raw material in a first vessel to a first temperature range, to produce a heated raw material wherein the solid phase raw material comprises from 80 to 90 percent by weight of tungsten hexachloride, and wherein a balance of the solid phase raw material comprises at least one impurity selected from the group consisting of molybdenum chloride, iron chloride, aluminum chloride, chromium chloride, nickel chloride, copper chloride, and tungsten oxytetrachloride. 5. The method of claim 1, wherein step a comprises heating the solid phase raw material in a first vessel to a first temperature range, to produce a heated raw material wherein the solid phase raw material comprises from 80 to 90 percent by weight of tungsten pentachloride, and wherein a balance of the solid phase raw material comprises at least one impurity selected from the group consisting of molybdenum chloride, iron chloride, aluminum chloride, chromium chloride, nickel chloride, copper chloride, and tungsten oxytetrachloride. 6. The method of claim 1, wherein step a comprises heating the solid phase raw material in a first vessel to a first temperature range, to produce a heated raw material wherein the first vessel comprises a sublimer and the first temperature range comprises a temperature range greater than a sublimation point of the tungsten chloride and less than the sublimation point of the at least one complexed impurity. 7. The method of claim 1, wherein step a comprises heating the solid phase raw material in a first vessel to a first temperature range, to produce a heated raw material wherein the first vessel is a smelter and the first temperature range comprises a temperature range greater than the melting point of the solid phase raw material. 8. The method of claim 1, wherein step b is performed in an absorption column. 9. The method of claim 1, wherein step b is performed in the first vessel. 10. The method of claim 8 wherein step c further comprises directing the second intermediate product to a process tool. 11. The method of claim 1 wherein step b further comprises contacting the heated raw material with a getter selected from the group consisting of potassium chloride and sodium chloride. 12. The method of claim 1, wherein step d further comprises wherein the second temperature range comprises a temperature range sufficient to cause the deposition of the second intermediate product to produce the product and to maintain the unreactive portion of the at least one impurity in a gaseous phase. 13. The method of claim 1, wherein step d further comprises separating the second intermediate product from the unreactive portion of the at least one impurity by cooling the second intermediate product to a second temperature range to produce a product, wherein the product comprises less than 10 parts per million by weight of all at least one impurity. 14. The method of claim 1, wherein step d further comprises separating the second intermediate product from the unreactive portion of the at least one impurity by cooling the second intermediate product to a second temperature range to produce a product, wherein the product comprises less than 5 parts per million by weight of all at least one impurity. 15. The method of claim 1, wherein step b further comprises: wherein the getter comprises a concentration, the concentration comprising at least 0.1 percent by weight of the solid phase raw material. 16. The method of claim 1, wherein the first pressure range comprises from 14.7 to 25 pounds per square inch absolute; the first temperature range comprises from 250 to 400 degrees Celsius and the second temperature range comprises from 130 to 250 degrees Celsius. 17. The method of claim 1, wherein the first pressure range comprises from 100 to 500 torr absolute; the first temperature range comprises from 200 to 300 degrees Celsius and the second temperature range comprises from 60 to 200 degrees Celsius. 18. The method of claim 1, wherein the first pressure range comprises less than 1 torr absolute; the first temperature range comprises from 130 to 250 degrees Celsius and the second temperature range comprises from 130 to 250 degrees Celsius. 19. A method of synthesizing high purity tungsten pentachloride, comprising: a.) adding a starting material comprising high purity tungsten hexachloride comprising less than 0.5 parts per million by combined weight of iron and molybdenum into a glass boiler container;b.) adding a getter selected from the group consisting of: potassium chloride; sodium chloride; rubidium chloride; cesium chloride; calcium chloride; magnesium chloride; barium chloride, and combinations thereof, in an amount equal to 0.1 to 10 percent by weight of the starting material;c.) heating the glass boiler container to 250 to 330 degrees Celsius to produce a tungsten hexachloride vapor;d.) directing a sweeping gas comprising at least 5 percent by volume of hydrogen in an inert gas into the glass boiler container at a flow rate sufficient to direct the tungsten hexachloride vapor into a tubular reactor heated to 400 degrees Celsius;e.) maintaining the flow rate sufficient to achieve a residence time of the tungsten hexachloride vapor in the tubular reactor to yield the conversion of the tungsten hexachloride vapor into a tungsten pentachloride vapor comprising less than 0.2 percent by weight of tungsten hexachloride;f.) condensing the tungsten pentachloride to yield a solid tungsten pentachloride composition. 20. A purified tungsten (VI) chloride composition comprising at least one impurity, wherein the composition comprises a concentration of iron less than 0.5 parts per million and a concentration of molybdenum less than 0.5 parts per million. 21. A system for purifying a solid phase raw material comprising tungsten hexachloride and at least one impurity comprising: a. at least one vessel adapted to heat the raw material causing vaporization and contact the vaporized raw material with a getter selected from the group consisting of: potassium chloride; sodium chloride; rubidium chloride; cesium chloride; calcium chloride; magnesium chloride; barium chloride, and combinations thereof;b. at least one separating vessel in fluid flow communication with the at least one vessel adapted to heat the raw materialc. at least one condenser in fluid flow communication with the at least one separating vessel. 22. The system for purifying a solid phase raw material comprising tungsten hexachloride and at least one impurity of claim 21 further comprising: at least one absorption column in fluid flow communication with the at least one vessel adapted to heat the raw material, and in fluid flow communication with the at least one separating vessel
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