METHOD AND APPARATUS FOR DECOMMISSIONING AND RECYCLING RETIRED ADSORBENT-BASED FLUID STORAGE AND DISPENSING VESSELS

Abstract

A method and apparatus for decommissioning a fluid storage and dispensing system including a fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid. The decommissioning involves removing the residual fluid, including superheating the adsorbent to temperature in a range of from (i) temperature substantially in excess of bulk desorption temperature of the fluid on the adsorbent, up to (ii) temperature substantially in excess of decomposition temperature of the fluid.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic representation of a decommissioning installation according to one embodiment of the invention.

FIG. 2 is a schematic representation of a decommissioning installation according to another embodiment of the invention.

FIG. 3 is a schematic representation of a decommissioning system according to another embodiment of the invention.

Claims

1. A method for decommissioning a fluid storage and dispensing system including a fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid, said method comprising removing said residual fluid, including superheating said adsorbent to temperature in a range of from (i) temperature substantially in excess of bulk desorption temperature of said fluid on said adsorbent, up to (ii) temperature substantially in excess of decomposition temperature of said fluid.

2. The method of claim 1, characterized by at least one of the following characteristics: (i) said residual fluid is removed at temperature of up to 600° C.;(ii) said fluid storage and dispensing system includes a valve head and said decommissioning includes removal of the valve head or a valve component thereof from the system;(iii) said decommissioning further includes recovery of the adsorbent from the vessel after removing said residual fluid therefrom;(iv) said fluid comprises arsine;(v) said superheating temperature includes temperature effective for decomposing residual fluid in said vessel;(vi) from 90 to 99 percent by weight of said residual fluid is removed from the vessel at temperature below the decomposition temperature of the residual fluid, whereby said residual fluid can be purified and reused;(vii) said fluid comprises arsine and said superheating temperature is effective to decompose arsine gas to hydrogen and arsenic;(viii) the vessel is heated to said superheating temperature by an external heating source;(ix) the vessel is heated to said superheating temperature by an external heating source, and said external heating source includes a heating source selected from the group consisting of electric furnaces, gas-fired furnaces, steam heating, liquid heat exchangers and inductive heaters;(x) the vessel is heated to said superheating temperature by an internal heating source;(xi) the vessel is heated to said superheating temperature by an internal heating source, and said internal heating source includes a heated gas injected into the vessel;(xii) the vessel is heated to said superheating temperature in a furnace;(xiii) the vessel is heated to said superheating temperature in a furnace, and at least one additional fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid is present in said furnace and heated to superheated temperature therein;(xiv) the vessel is heated to said superheating temperature in a furnace, and the vessel in said furnace is coupled in gas flow communication with flow circuitry including a manifold, and wherein said manifold is coupled in flow communication with a residual fluid recovery or destruction system;(xv) the vessel is heated to said superheating temperature in a furnace, and the vessel in said furnace is coupled in gas flow communication with flow circuitry including a manifold, and wherein said manifold is coupled in flow communication with a residual fluid recovery or destruction system, and a pump is coupled to the flow circuitry to pump the residual fluid to the residual fluid recovery or destruction system;(xvi) the residual fluid comprises fluid selected from the group consisting of arsine, boron trifluoride, silicon tetrafluoride, germanium tetrafluoride, phosphine, arsine, arsenic pentafluoride, phosphorus pentafluoride, and hydrogen selenide;(xvii) removing said residual fluid comprises multiple stages of heat ramping and/or heat soaking;(xviii) removing said residual fluid comprises multiple stages of heat ramping and/or heat soaking, wherein said multiple stages are conducted so as to control rate of desorption of the residual fluid from the adsorbent, to avoid thermal runaway reaction and to maximize amount of fluid that is desorbed to amount of fluid that is decomposed;(xix) removing said residual fluid comprises initial heating to temperature in a range of from about 25° C. to about 200° C., followed by heating to higher temperature at which decomposition is a primary removing modality of said residual fluid;(xx) removing said residual fluid comprises initial heating to temperature in a range of from about 25° C. to about 200° C., followed by heating to higher temperature at which decomposition is a primary removing modality of said residual fluid, wherein said fluid storage and dispensing system includes a valve head and a valve in said valve head is open during said initial heating, and closed at onset of decomposition of the residual fluid in the vessel;(xxi) removing said residual fluid comprises initial heating to temperature in a range of from about 25° C. to about 200° C., followed by heating to higher temperature at which decomposition is a primary removing modality of said residual fluid, wherein said fluid storage and dispensing system includes a valve head and a valve in said valve head is open during said initial heating, and closed at onset of decomposition of the residual fluid in the vessel, further comprising monitoring the residual fluid removed from said fluid storage and dispensing vessel to determine said onset of decomposition, and thereupon responsively closing said valve in said valve head;(xxii) said monitoring comprises use of a fluid analyzer adapted to sense at least one decomposition product of said residual fluid removed from said fluid storage and dispensing vessel;(xxiii) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid;(xxiv) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, wherein said manifold contains flow control valves;(xxv) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, wherein said manifold contains flow control valves, wherein said manifold is coupled with a vacuum system adapted to remove residual fluid from said fluid storage and dispensing vessel during said removing;(xxvi) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, wherein said manifold contains flow control valves, wherein said manifold is coupled with a vacuum system adapted to remove residual fluid from said fluid storage and dispensing vessel during said removing, wherein said vacuum system comprises a vacuum extractor selected from the group consisting of oil-based rotary pumps, mechanical dry pumps, diaphragm pumps, cold traps and cryogenic pumps;(xxvii) said adsorbent comprises a sorbent medium selected from the group consisting of solid adsorbents, liquid adsorbents, and semi-solid adsorbents;(xxviii) said adsorbent comprises a carbon material;(xxix) said adsorbent comprises an ionic liquid medium;(xxx) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, wherein said manifold contains flow control valves, wherein said manifold is coupled with a vacuum system adapted to remove residual fluid from said fluid storage and dispensing vessel during said removing, and said manifold is coupled with a source of purge fluid and said valves are selectively actuatable to flow purge fluid into said fluid storage and dispensing vessel;(xxxi) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, wherein said manifold is coupled with a scrubber selected from the group consisting of wet scrubbers and dry scrubbers; and(xxxii) said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, wherein said manifold is coupled to at least one additional fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid.

3. The method of claim 1, wherein said fluid storage and dispensing vessel is contained in a furnace adapted to heat said vessel during said superheating.

4. The method of claim 1, comprising introducing purge fluid into said fluid storage and dispensing vessel during said superheating.

5. The method of claim 4, wherein said purge fluid is extracted from said fluid storage and dispensing vessel by vacuum extraction during said superheating.

6. The method of claim 5, wherein repetitive purge fluid fill and extraction steps are conducted during said superheating.

7. The method of claim 1, wherein said fluid storage and dispensing vessel is maintained in a closed condition during a portion of said superheating, followed by opening of said vessel for said removing.

8. The method of claim 1, wherein said fluid storage and dispensing vessel is connected to a manifold adapted for said removing of said residual fluid, and the removed residual fluid is recirculated through the manifold.

10. The method of claim 1, further comprising processing the removed residual fluid by a process selected from among: scrubbing; treatment in a fluid destruction system; solids-removal treatment; cryogenic cooling to recover the removed residual fluid; purification of the removed residual fluid.

11. The method of claim 1, wherein fluid removed from said fluid storage and dispensing vessel includes residual fluid and purge fluid.

12. An apparatus for decommissioning a fluid storage and dispensing system including a fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid, said apparatus comprising a heater adapted to superheat said adsorbent in said fluid storage and dispensing vessel to remove said residual fluid from the adsorbent, flow circuitry coupled to said fluid storage and dispensing vessel, a purge fluid source coupled to said flow circuitry, said flow circuitry containing flow control valves therein, said flow control valves being selectively actuatable to flow purge fluid from said purge fluid source through said flow circuitry into said fluid storage and dispensing vessel, a pump connected to said flow circuitry and adapted to extract said residual fluid from said fluid storage and dispensing vessel, and a scrubber connected to said flow circuitry and adapted to scrub fluid flowed thereto from the flow circuitry.

13. The apparatus of claim 12, characterized by at least one of the following characteristics: (i) the heater comprises a furnace adapted to hold the fluid storage and dispensing vessel;(ii) the heater comprises a furnace adapted to hold the fluid storage and dispensing vessel, and the furnace is adapted to hold at least one additional fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid;(iii) said flow circuitry comprises a manifold and branch lines interconnecting the manifold with each fluid storage and dispensing vessel in the furnace;(iv) said flow circuitry is coupled with a solids collector adapted to remove solids from fluid removed from said fluid storage and dispensing vessel;(v) said flow circuitry is coupled with a cryogenic fluid recovery trap adapted to recover the residual fluid;(vi) said flow circuitry is coupled with a fluid purification system;(vii) said flow circuitry is coupled with a residual fluid recovery container for collection of the residual fluid;(viii) said flow circuitry is coupled with a fluid purification system, and the flow circuitry is coupled with a residual fluid recovery container for collection of residual fluid subsequent to purification thereof in the fluid purification system;(viii) said flow circuitry is coupled with a solids collector, a cryogenic fluid recovery trap, a fluid purification system, and a purified fluid receiver container;(ix) said heater is adapted to superheat said adsorbent to temperature in a range of from (i) temperature substantially in excess of bulk desorption temperature of said fluid on said adsorbent, up to (ii) temperature substantially in excess of decomposition temperature of said fluid;(x) said residual fluid comprises arsine;(xi) said heater is adapted to superheat said adsorbent to temperature effective for decomposing residual fluid in said vessel;(xii) said residual fluid comprises arsine, and said heater is adapted to superheat said adsorbent to temperature effective to decompose arsine to hydrogen and arsenic;(xiii) said heater comprises an external heating source selected from among electric furnaces, gas-fired furnaces, steam heating, liquid heat exchangers and inductive heaters;(xiv) said heater comprises an internal heating source;(xv) said heater comprises an internal heating source including a heated fluid injected into the vessel;(xvi) the apparatus is adapted for processing of at least one additional fluid storage and dispensing vessel containing adsorbent sorptively retaining residual fluid;(xvii) said heater comprises a furnace, and said fluid storage and dispensing vessel is contained in said furnace, and said flow circuitry is coupled in flow communication with a residual fluid recovery or destruction system;(xviii) said residual fluid in said fluid storage and dispensing vessel comprises fluid selected from the group consisting of arsine, boron trifluoride, silicon tetrafluoride, germanium tetrafluoride, phosphine, arsine, arsenic pentafluoride, phosphorus pentafluoride, and hydrogen selenide;(xix) said heater is adapted to conduct multiple stages of heat ramping and/or heat soaking;(xx) said heater is adapted to conduct multiple stages of heat ramping and/or heat soaking, wherein said heater is adapted to control rate of desorption of the residual fluid from the adsorbent, to avoid thermal runaway reaction and to maximize amount of fluid that is desorbed to amount of fluid that is decomposed;(xxi) said heater is adapted to initially heat said adsorbent to temperature in a range of from about 25° C. to about 200° C., followed by heating to higher temperature at which decomposition is a primary removing modality to remove said residual fluid from said adsorbent;(xxii) said heater is adapted to initially heat said adsorbent to temperature in a range of from about 25° C. to about 200° C., followed by heating to higher temperature at which decomposition is a primary removing modality to remove said residual fluid from said adsorbent, and said fluid storage and dispensing system includes a valve head and a valve in said valve head that is openable during the initial heating, and closable at onset of decomposition of the residual fluid in the vessel;(xxiii) said heater is adapted to initially heat said adsorbent to temperature in a range of from about 25° C. to about 200° C., followed by heating to higher temperature at which decomposition is a primary removing modality to remove said residual fluid from said adsorbent, and said fluid storage and dispensing system includes a valve head and a valve in said valve head that is openable during the initial heating, and closable at onset of decomposition of the residual fluid in the vessel, said apparatus further comprising a residual fluid monitor adapted to determine said onset of decomposition, and thereupon responsively actuate closure of said valve in said valve head;(xxiv) said pump comprises a vacuum system adapted to remove residual fluid from said fluid storage and dispensing vessel, wherein said pump is selected from among oil-based rotary pumps, mechanical dry pumps, diaphragm pumps, cold traps and cryogenic pumps;(xxv) said adsorbent comprises a sorbent medium selected from the group consisting of solid adsorbents, liquid adsorbents, and semi-solid adsorbents;(xxvi) said adsorbent comprises a carbon material;(xxvii) said adsorbent comprises an ionic liquid medium;(xxviii) said scrubber is selected from among wet scrubbers and dry scrubbers;(xxix) said flow circuitry is adapted for recirculation of at least a portion of the residual fluid after removal thereof from the fluid storage and dispensing vessel; and(xxx) said fluid storage and dispensing vessel comprises an interior fluid pressure regulator.

14. The method of claim 1, wherein the adsorbent sorptively retaining residual fluid is removed from the fluid storage and dispensing vessel, wherein the vessel during such removal is in a containment zone, whereby the vessel is isolated from an ambient environment exterior to the containment zone during said removal.

15. The method of claim 14, characterized by at least one of the following: (i) the containment zone comprises a glove box;(ii) the adsorbent superheating is conducted in a thermal desorption zone that is in or connected to the containment zone; and(iii) the adsorbent superheating is conducted in a thermal desorption zone that is in or connected to the containment zone, and an adsorbent collection container is disposed in the thermal desorption zone, and after removal of the valve head from the vessel, adsorbent is transferred from the fluid storage and dispensing vessel to the adsorbent collection container.

16. The method of claim 1, comprising removing adsorbent from said fluid storage and dispensing vessel.

17. The method of claim 16, comprising establishing an open material removal port in said fluid storage and dispensing vessel to enable adsorbent to be removed therefrom, wherein the open material removal port is established by opening a preexisting openable material removal port, or by drilling or tapping an opening in said fluid storage and dispensing vessel.

18. The method of claim 1, wherein said residual fluid comprises a fluid selected from among arsine and phosphine.

19. The method of claim 1, wherein the removed residual fluid is processed in a fluid purification system adapted to purify said removed residual fluid to a purity greater than 99.9 wt. %.

20. The method of claim 19, wherein purified fluid produced by said fluid purification system is introduced to a fresh fluid storage and dispensing vessel containing adsorbent that is sorptive of said purified fluid.

21. The method of claim 1, further comprising, after removing said residual fluid, introducing into the fluid storage and dispensing vessel a reactive fluid to react with vestigial adsorbed fluid remaining on said adsorbent for neutralization thereof.

22. The method of claim 21, wherein the reaction product of reaction of the reactive fluid and the vestigial adsorbed fluid is a non-volatile reaction product.

23. The apparatus of claim 12, further comprising a residual fluid purity monitor arranged to monitor purity of residual fluid, and to responsively actuate flow of the residual fluid to one of a purification system and a disposal system, depending on purity of the residual fluid as being within a first range amenable to purification in said purification system, or as being within a second range inconsistent with purification in said purification system and consistent with disposition by said disposal system.

24. A method of manufacturing a microelectronic device, comprising use of a fluid produced by purification of a residual fluid removed from a fluid storage and dispensing system decommissioned by the method of claim 1.

25. A method of fabricating a fluid storage and dispensing system, comprising introducing to a fluid storage and dispensing vessel residual fluid removed from a fluid storage and dispensing system decommissioned by the method of claim 1, wherein said fluid storage and dispensing vessel contains adsorbent on which said residual fluid is adsorbed, and sealing the fluid storage and dispensing vessel for storage of the introduced fluid therein.

26. A method of recycling a semiconductor manufacturing fluid, comprising decommissioning a fluid storage and dispensing system containing said semiconductor manufacturing fluid as residual fluid, according to the method of claim 1, and utilizing the residual fluid in a semiconductor manufacturing process.

27. The method of claim 26, wherein the semiconductor manufacturing fluid comprises one of arsine and phosphine, and the semiconductor manufacturing process comprises ion implantation.

28. The apparatus of claim 12, further comprising a supply of reactive fluid coupled to the flow circuitry and arranged to flow said reactive fluid into the fluid storage and dispensing vessel, after removal of said residual fluid therefrom, for reaction with vestigial adsorbed fluid remaining on said adsorbent for neutralization thereof.

29. A decommissioned fluid storage and dispensing apparatus, including a physical sorbent superheated to remove a residual fluid, with the physical sorbent having removed therefrom traces of a toxic gas.

30. A decommissioned fluid storage and dispensing vessel containing a physical adsorbent having residual sorbate fluid thereon, in an impermeable encasement medium.

31. The decommissioned fluid storage and dispensing vessel according to claim 30, wherein the impermeable encasement medium comprises a vitreous material.

32. The method of claim 1, wherein residual fluid is removed by introducing into the fluid storage and dispensing vessel a reactive fluid that reacts with the residual fluid.

33. The method of claim 32, wherein the reaction product of reaction of the reactive fluid and the residual fluid is a non-volatile reaction product.

34. The method of claim 1, wherein prior to removing said residual fluid, the fluid storage and dispensing vessel being decommissioned comprises a used fluid storage and dispensing vessel that contains more than said residual fluid, and said used vessel is coupled in flow communication with at least one fresh storage and dispensing vessel containing sorbent material therein having sorptive capacity for said fluid, with the fresh vessel being maintained at temperature and/or pressure conditions relative to the used vessel that cause fluid to be transferred from the used vessel to the fresh vessel, so that the used vessel subsequent to such transfer contains said residual fluid.