Methods are described for filling gas mixture supply vessels with constituent gases to achieve precision compositions of the gas mixture, wherein the gas mixture comprises at least two constituent gases. Cascading fill techniques may be employed, involving flowing of gases from single source vessels
Methods are described for filling gas mixture supply vessels with constituent gases to achieve precision compositions of the gas mixture, wherein the gas mixture comprises at least two constituent gases. Cascading fill techniques may be employed, involving flowing of gases from single source vessels to multiple target vessels, or from multiple source vessels to a single target vessel. The methods may be employed to form dopant gas mixtures, e.g., of boron trifluoride and hydrogen, for ion implantation applications.
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1. A method of filling gas mixture supply vessels with constituent gases to achieve precision compositions of the gas mixture, wherein said gas mixture comprises at least two constituent gases, said method comprising: (A) providing a source vessel of a constituent first gas comprising dopant gas, an
1. A method of filling gas mixture supply vessels with constituent gases to achieve precision compositions of the gas mixture, wherein said gas mixture comprises at least two constituent gases, said method comprising: (A) providing a source vessel of a constituent first gas comprising dopant gas, and multiple target vessels to be filled with said at least two constituent gases;(B) flowing the constituent first gas to at least one of the multiple target vessels for a period of time until a predetermined pressure is reached or until pressure stabilizes;(C) discontinuing flow of the constituent first gas to said at least one of the multiple target vessels, comprising closing said at least one of the multiple target vessels to which constituent first gas has been flowed;(D) repeating steps (A)-(C) for each of other ones of the multiple target vessels to which constituent first gas has not been introduced;(E) closing the source vessel;(F) optionally repeating steps (A)-(E) with one or more other source vessels of the constituent first gas until a predetermined target pressure of the constituent first gas is reached in said multiple target vessels, to provide constituent first gas in said multiple target vessels at said predetermined target pressure; and(G) introducing a constituent second gas to each of the target vessels to form said gas mixture, the constituent second gas comprising a supplemental gas that is not a dopant gas, the constituent second gas being added to achieve a total transient pressure that corresponds to known relative proportions of the constituent gases, wherein the constituent first gas comprises a heaviest gas of the constituent gases in the gas mixture. 2. The method according to claim 1, wherein only one source vessel and one target vessel are in open gas flow communication with one another at any time when the constituent first gas is flowed from a source vessel to a target vessel. 3. The method according to claim 1, wherein the target vessels comprise gas cylinders. 4. The method according to claim 1, wherein the source vessel is at higher pressure than the target vessels. 5. The method according to claim 1, wherein the source vessel is at lower pressure than the target vessels, further comprising pressurizing the constituent first gas to form pressurized constituent first gas for flow to one of the multiple target vessels, wherein said pressurizing is conducted by a pressurization process selected from the group consisting of: (i) a first pressurization process comprising mechanical gas compression of the constituent first gas;(ii) a second pressurization process comprising collecting the constituent first gas in an intermediate vessel, cooling the constituent first gas to at least partially condense same, and warming the at least partially condensed constituent first gas to increase pressure thereof;(iii) a third pressurization process comprising collecting the constituent first gas in an intermediate vessel, and heating the constituent first gas to increase pressure thereof; and(iv) a fourth pressurization process comprising heating the first source vessel containing the constituent first gas. 6. The method according to claim 1, further comprising thermally controlling said target vessels after fill thereof with constituent first gas, for subsequent fill with other(s) of said constituent gases. 7. The method according to claim 6, further comprising maintaining the target vessel at predetermined temperature during introduction of said other(s) of said constituent gases to the target vessel. 8. The method according to claim 7, wherein said other(s) of said constituent gases is/are at predetermined pressure during their introduction to the target vessel. 9. The method of claim 8, wherein at least one of said other(s) of said constituent gases is at a predetermined pressure for the gas mixture, so that completion of gas fill of the vessel with said other(s) of said constituent gases provides the gas mixture in said vessel at said predetermined pressure. 10. The method according to claim 1, wherein the gas mixture comprises boron trifluoride and hydrogen. 11. The method according to claim 1, wherein the dopant gas is selected from the group consisting of germanium tetrafluoride, germane, boron trifluoride, diborane, diboron tetrafluoride, silicon tetrafluoride, silane, carbonyl difluoride, arsine, hydrogen selenide, hydrogen sulfide, phosphine, boron trichloride, and xenon difluoride. 12. The method according to claim 1, wherein a source vessel contains a pre-mixed gas composition, and the method is conducted to yield a predetermined gas mixture composition therefrom. 13. The method according to claim 1, comprising automated operation of at least one step of the method. 14. The method of claim 1 wherein the constituent second gas is a supplemental gas selected from argon, neon, xenon, hydrogen, fluorine, oxygen, nitrogen, and helium. 15. The method of claim 1 wherein the dopant gas is selected from germanium tetrafluoride, boron trifluoride, and silicon tetrafluoride. 16. The method of claim 15 wherein the constituent second gas is hydrogen. 17. The method of claim 1 wherein the total pressure upon addition of the constituent second gas is determined empirically.
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