IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0315635
(2002-12-10)
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발명자
/ 주소 |
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출원인 / 주소 |
- Advanced Technology Materials, Inc.
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대리인 / 주소 |
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인용정보 |
피인용 횟수 :
39 인용 특허 :
37 |
초록
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A fluid storage and dispensing apparatus, including a fluid storage and dispensing vessel having an interior volume, in which the interior volume contains a physical adsorbent sorptively retaining a fluid thereon and from which the fluid is desorbable for dispensing from the vessel, and a dispensing
A fluid storage and dispensing apparatus, including a fluid storage and dispensing vessel having an interior volume, in which the interior volume contains a physical adsorbent sorptively retaining a fluid thereon and from which the fluid is desorbable for dispensing from the vessel, and a dispensing assembly coupled to the vessel for dispensing desorbed fluid from the vessel. The physical adsorbent includes a monolithic carbon physical adsorbent that is characterized by at least one of the following characteristics: (a) a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is greater than 400 grams arsine per liter of adsorbent; (b) at least 30% of overall porosity of the adsorbent including slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity including micropores of diameter <2 nanometers; and (c) having been formed by pyrolysis and optional activation, at temperature(s) below 1000° C., and having a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter.
대표청구항
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1. A method of storing and dispensing a gas, comprising: fabricating a gas storage and dispensing vessel; disposing a physical adsorbent in the vessel having sorptive affinity for said gas; charging said gas to said vessel for adsorption on said physical adsorbent; sealing said vessel with a valve h
1. A method of storing and dispensing a gas, comprising: fabricating a gas storage and dispensing vessel; disposing a physical adsorbent in the vessel having sorptive affinity for said gas; charging said gas to said vessel for adsorption on said physical adsorbent; sealing said vessel with a valve head containing an actuatable valve, to enclose the physical adsorbent and adsorbed gas, and isolate same from an exterior environment of the vessel; desorbing the adsorbed gas from the physical adsorbent, and actuating the actuatable valve in the valve head, to flow gas from the vessel and through the actuatable valve, for gas dispensing; wherein the physical adsorbent is characterized by at least one of the following characteristics: (a) a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is greater than 400 grams arsine per liter of adsorbent; (b) at least 30% of overall porosity of said adsorbent comprising slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity comprising micropores of diameter <2 nanometers; and (c) a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter. 2. The method of claim 1, wherein the adsorbent has a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is greater than 400 grams arsine per liter of adsorbent.3. The method of claim 1, wherein at least 30% of overall porosity of said adsorbent comprises slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity comprises micropores of diameter <2 nanometers.4. The method of claim 1, wherein said adsorbent has a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter.5. The method of claim 1, wherein said physical adsorbent comprises pyrolyzed PVDC.6. The method of claim 5, wherein the pyrolyzed PVDC has been subjected to activation conditions.7. The method of claim 6, wherein the activation conditions comprise exposure of the pyrolyzed PVDC to an elevated temperature non-oxidizing environment, followed by exposure of the pyrolyzed PVDC to an elevated temperature oxidizing environment.8. The method of claim 1, wherein said fill density measured for arsine gas at 25° C. and pressure of 650 torr is greater than 450 grams arsine per liter of adsorbent.9. The method of claim 1, wherein the gas comprises a gas selected from the group consisting of arsine, phosphine, hydrogen selenide, hydrogen telluride, nitrogen trifluoride, boron trifluoride, boron trichloride, diborane, trimethylsilane, tetramethylsilane, disilane, silane, germane, and organometallic gaseous reagents.10. A fluid storage and dispensing apparatus, comprising a fluid storage and dispensing vessel having an interior volume, wherein the interior volume contains a physical adsorbent sorptively retaining a fluid thereon and from which the fluid is desorbable for dispensing from the vessel, and a dispensing assembly coupled to the vessel for dispensing desorbed fluid from the vessel, wherein the physical adsorbent comprises a monolithic carbon physical adsorbent that is characterized by at least one of the following characteristics: (a) a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is greater than 400 grams arsine per liter of adsorbent; (b) at least 30% of overall porosity of said adsorbent comprising slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity comprising micropores of diameter <2 nanometers; and (c) having been formed by pyrolysis and optional activation, at temperature(s) below 1000° C., and having a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter. 11. The fluid storage and dispensing apparatus of claim 10, wherein the adsorbent has a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is gre ater than 400 grams arsine per liter of adsorbent.12. The fluid storage and dispensing apparatus of claim 10, wherein at least 30% of overall porosity of said adsorbent comprises slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity comprises micropores of diameter <2 nanometers.13. The fluid storage and dispensing apparatus of claim 10, wherein said adsorbent has been formed by pyrolysis and optional activation, at temperature(s) below 1000° C., and has a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter.14. The fluid storage and dispensing apparatus of claim 10, wherein said adsorbent has a monolithic form that is selected from the group consisting of blocks, bricks, and boules.15. The fluid storage and dispensing apparatus of claim 14, wherein the monolithic form comprises a single monolithic article.16. The fluid storage and dispensing apparatus of claim 14, wherein the monolithic form comprises a multiplicity of discrete monolithic articles.17. The fluid storage and dispensing apparatus of claim 16, wherein the interior volume of the vessel contains less than 75 discrete monolithic articles of said physical adsorbent.18. The fluid storage and dispensing apparatus of claim 16, wherein the interior volume of the vessel contains less than 20 discrete monolithic articles of said physical adsorbent.19. The fluid storage and dispensing apparatus of claim 16, wherein the interior volume of the vessel contains less than 8 discrete monolithic articles of said physical adsorbent.20. The fluid storage and dispensing apparatus of claim 16, wherein the interior volume of the vessel contains less than 4 discrete monolithic articles of said physical adsorbent.21. The fluid storage and dispensing apparatus of claim 16, wherein each of the multiplicity of discrete monolithic articles has a rectangular parallelepiped shape.22. The fluid storage and dispensing apparatus of claim 16, wherein each of the multiplicity of discrete monolithic articles is laterally and/or longitudinally abutted in surface contact with adjacent monolithic members in the interior volume of the vessel.23. The fluid storage and dispensing apparatus of claim 16, wherein each of the multiplicity of discrete monolithic articles has a solid cylinder form.24. The fluid storage and dispensing apparatus of claim 16, wherein each of the multiplicity of discrete monolithic articles has a length to cross-sectional dimension ratio, L/D, that is from about 2 to about 20, where L is the length or major axis dimension of the monolithic carbon sorbent article, and D is the transverse or minor axis dimension.25. The fluid storage and dispensing apparatus of claim 16, wherein each of the multiplicity of discrete monolithic articles has a length to cross-sectional dimension ratio, L/D, that is from about 4 to about 15, where L is the length or major axis dimension of the monolithic carbon sorbent article, and D is the transverse or minor axis dimension.26. The fluid storage and dispensing apparatus of claim 10, wherein the monolithic physical adsorbent provides a sorbent mass that is conformed in size and shape to the interior volume of the vessel.27. The fluid storage and dispensing apparatus of claim 26, wherein the sorbent mass occupies at least 60% of the interior volume of the vessel.28. The fluid storage and dispensing apparatus of claim 26, wherein the sorbent mass occupies from about 75% to about 95% of the interior volume of the vessel.29. The fluid storage and dispensing apparatus of claim 10, wherein the adsorbent is a pyrolysis product of an organic resin.30. The fluid storage and dispensing apparatus of claim 29, wherein the adsorbent has been formed in situ in the vessel.31. The fluid storage and dispensing apparatus of claim 10, wherein the adsorbent is a pyrolysis product of a polymer selected from the group consisting of polyvinylidene chloride, phenol-formaldehyde resins, polyfurfuryl alcohol, coconut shells, peanut shells, peach pits, olive stones, polyacrylonitrile, and polyacrylamide.32. The fluid storage and dispensing apparatus of claim 10, wherein the adsorbent comprises a multiplicity of discrete monolithic adsorbent articles, wherein each of the multiplicity of discrete monolithic adsorbent articles has a length that is between 0.3 and 1.0 times the height of the interior volume of the vessel, and a cross-sectional area that is between 0.1 and 0.5 times the rectangular cross-sectional area of the vessel.33. The fluid storage and dispensing apparatus of claim 10, wherein said adsorbent comprises pyrolyzed PVDC resin.34. The fluid storage and dispensing apparatus of claim 10, wherein said adsorbent has a doping agent thereon.35. The fluid storage and dispensing apparatus of claim 34, wherein said doping agent comprises at least one agent selected from the group consisting of boric acid, sodium tetraborate, sodium silicate, and disodium hydrogen phosphate.36. The fluid storage and dispensing apparatus of claim 35, wherein the vessel comprises a metal material of construction.37. The fluid storage and dispensing apparatus of claim 36, wherein said metal is selected from the group consisting of steel, stainless steel, aluminum, copper, brass, bronze, and alloys thereof.38. The fluid storage and dispensing apparatus of claim 37, wherein the fluid comprises boron trifluoride.39. The fluid storage and dispensing apparatus of claim 10, wherein the fluid comprises a fluid having utility in semiconductor manufacturing.40. The fluid storage and dispensing apparatus of claim 10, wherein the fluid comprises a fluid selected from the group consisting of hydrides, halides and organometallic gaseous reagents.41. The fluid storage and dispensing apparatus of claim 10, wherein the fluid comprises a fluid selected from the group consisting of silane, germane, arsine, phosphine, phosgene, diborane, germane, ammonia, stibine, hydrogen sulfide, hydrogen selenide, hydrogen telluride, nitrous oxide, hydrogen cyanide, ethylene oxide, deuterated hydrides, halide (chlorine, bromine, fluorine, and iodine) compounds, and organometallic compounds.42. The fluid storage and dispensing apparatus of claim 10, wherein the fluid has a pressure in said interior volume not exceeding about 2500 torr.43. The fluid storage and dispensing apparatus of claim 10, wherein the fluid has a pressure in said interior volume not exceeding about 2000 torr.44. The fluid storage and dispensing apparatus of claim 10, wherein the fluid has a pressure in said interior volume in a range of from about 20 to about 1800 torr.45. The fluid storage and dispensing apparatus of claim 10, wherein the fluid has a pressure in said interior volume in a range of from about 20 to about 1200 torr.46. The fluid storage and dispensing apparatus of claim 10, wherein the fluid has a subatmospheric pressure in said interior volume.47. The fluid storage and dispensing apparatus of claim 10, wherein the fluid has a pressure in said interior volume in a range of from about 20 to about 750 torr.48. The fluid storage and dispensing apparatus of claim 10, wherein the vessel comprises a material of construction selected from the group consisting of metals, glasses, ceramics, vitreous materials, polymers, and composite materials.49. The fluid storage and dispensing apparatus of claim 10, wherein the adsorbent has at least 20% of its porosity in pores with a diameter of less than 2 nanometers.50. The fluid storage and dispensing apparatus of claim 10, wherein the vessel has a rectangular parallelepiped shape.51. The fluid storage and dispensing apparatus of claim 10, wherein the vessel has an elongate shape with a square cross-section.52. The fluid storage and dispensing apparatus of claim 10, wherein the vessel has a cylindrical shape.53. A method of forming a monolithic adsorbent for use in a gas storage and dispensing system, said method comprising: molding a pyrolyza ble material into a monolithic shape; and pyrolyzing the pyrolyzable material under pyrolysis conditions producing a monolithic adsorbent that is characterized by at least one of the following characteristics: (a) a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is greater than 400 grams arsine per liter of adsorbent; (b) at least 30% of overall porosity of said adsorbent comprising slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity comprising micropores of diameter <2 nanometers; and (c) a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter, wherein said pyrolysis conditions comprise temperature below 1000° C. 54. The method of claim 53, wherein the adsorbent has a fill density measured for arsine gas at 25° C. and pressure of 650 torr that is greater than 400 grams arsine per liter of adsorbent.55. The method of claim 53, wherein at least 30% of overall porosity of said adsorbent comprises slit-shaped pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 20% of the overall porosity comprises micropores of diameter <2 nanometers.56. The method of claim 53, wherein said pyrolysis conditions comprise temperature below 1000° C., and said adsorbent has a bulk density of from about 0.80 to about 2.0 grams per cubic centimeter.57. The method of claim 53, wherein said adsorbent has a monolithic form that is selected from the group consisting of blocks, bricks, and boules.58. The method of claim 53, further comprising activating said adsorbent.59. The method of claim 58, wherein said activating comprises exposure of said adsorbent to a non-oxidizing environment at elevated temperature, followed by exposure of said adsorbent to an oxidizing environment.60. The method of claim 59, wherein said non-oxidizing environment comprises nitrogen.61. The method of claim 59, wherein said oxidizing environment comprises carbon dioxide.62. The method of claim 59, wherein said oxidizing environment comprises steam.63. The method of claim 59, wherein the adsorbent is cooled in a non-oxidizing environment after said exposure to said oxidizing environment.64. The method of claim 53, wherein said adsorbent comprises a single monolithic article.65. The method of claim 64, further comprising disposing said adsorbent in a gas storage and dispensing vessel; charging to the vessel a gas for which the adsorbent has sorptive affinity, to adsorb said gas thereon; sealing said vessel to enclose said adsorbent holding adsorbed gas thereon in an interior volume of the vessel; and coupling the vessel to a dispensing assembly for dispensing desorbed fluid from the vessel.66. The method of claim 65, wherein said adsorbent article is conformed in size and shape to the interior volume of the vessel.67. The method of claim 65, wherein said adsorbent article occupies at least 60% of the interior volume of the vessel.68. The method of claim 65, wherein said adsorbent article occupies from about 75% to about 95% of the interior volume of the vessel.69. The method of claim 53, wherein said adsorbent comprises a multiplicity of discrete monolithic articles.70. The method of claim 69, further comprising disposing said adsorbent in a gas storage and dispensing vessel; charging to the vessel a gas for which the adsorbent has sorptive affinity, to adsorb said gas thereon; sealing said vessel to enclose said adsorbent holding adsorbed gas thereon in an interior volume of the vessel; and coupling the vessel to a dispensing assembly for dispensing desorbed fluid from the vessel.71. The method of claim 70, wherein the interior volume of the vessel contains less than 75 discrete monolithic articles of said adsorbent.72. The method of claim 70, wherein the interior volume of the vessel contains less than 20 discrete monolithic articles of said adsorbent.73. The method of claim 70, wherein the interior volume of the vessel contains less than 8 discrete monolithic articles of said adsorbent.74. The method of claim 70, wherein the interior volume of the vessel contains less than 4 discrete monolithic articles of said adsorbent.75. The method of claim 70, wherein said adsorbent provides a sorbent mass that is conformed in size and shape to the interior volume of the vessel.76. The method of claim 75, wherein the sorbent mass occupies at least 60% of the interior volume of the vessel.77. The method of claim 75, wherein the sorbent mass occupies from about 75% to about 95% of the interior volume of the vessel.78. The method of claim 70, wherein each of said discrete monolithic articles has a length that is between 0.3 and 1.0 times the height of the interior volume of the vessel, and a cross-sectional area that is between 0.1 and 0.5 times the cross-sectional area of the interior volume of the vessel.79. The method of claim 70, wherein each of said discrete monolithic articles has a rectangular parallelepiped shape.80. The method of claim 79, wherein each of the multiplicity of discrete monolithic articles is laterally and/or longitudinally abutted in surface contact with adjacent monolithic members in the interior volume of the vessel.81. The method of claim 79, wherein each of the multiplicity of discrete monolithic articles has a solid cylinder form.82. The method of claim 79, wherein each of the multiplicity of discrete monolithic articles has a length to cross-sectional dimension ratio, LID, that is from about 2 to about 20, where L is the length or major axis dimension of the monolithic carbon sorbent article, and D is the transverse or minor axis dimension.83. The method of claim 79, wherein each of the multiplicity of discrete monolithic articles has a length to cross-sectional dimension ratio, LID, that is from about 4 to about 15, where L is the length or major axis dimension of the monolithic carbon sorbent article, and D is the transverse or minor axis dimension.84. The method of claim 53, wherein the pyrolyzable material comprises an organic resin.85. The method of claim 53, wherein the pyrolyzable material comprises a material selected from the group consisting of polyvinylidene chloride, phenol-formaldehyde resins, polyfurfuryl alcohol, coconut shells, peanut shells, peach pits, olive stones, polyacrylonitrile, and polyacrylamide.86. The method of claim 53, wherein the pyrolyzable material is pyrolyzed in situ in a gas storage and dispensing vessel of said gas storage and dispensing system.87. The method of claim 53, wherein said pyrolyzable material comprises PVDC resin.88. The method of claim 53, further comprising doping said adsorbent with a doping agent.89. The method of claim 88, wherein said doping agent comprises at least one agent selected from the group consisting of boric acid, sodium tetraborate, sodium silicate, and disodium hydrogen phosphate.90. The method of claim 53, further comprising disposing said adsorbent in a gas storage and dispensing vessel; charging to the vessel a gas for which the adsorbent has sorptive affinity, to adsorb said gas thereon; sealing said vessel to enclose said adsorbent holding adsorbed gas thereon in an interior volume of the vessel; and coupling the vessel to a dispensing assembly for dispensing desorbed fluid from the vessel.91. The method of claim 90, wherein the gas comprises a gas having utility in semiconductor manufacturing.92. The method of claim 90, wherein the gas comprises a gas selected from the group consisting of hydrides, halides and organometallic gaseous reagents.93. The method of claim 90, wherein the gas comprises a gas selected from the group consisting of silane, germane, arsine, phosphine, phosgene, diborane, germane, ammonia, stibine, hydrogen sulfide, hydrogen selenide, hydrogen telluride, nitrous oxide, hydrogen cyanide, ethylene oxide, deuterated hydrides, halide (chlorine, bromine, fluorine, and iodine) compounds, and organometallic compounds.94. The method of claim 90, wherein the gas has a pressure in said interior volume not exceeding about 2500 torr.95. The method of claim 90, wherein the gas has a pressure in said interior volume not exceeding about 2000 torr.96. The method of claim 90, wherein the gas has a pressure in said interior volume in a range of from about 20 to about 1800 torr.97. The method of claim 90, wherein the gas has a pressure in said interior volume in a range of from about 20 to about 1200 torr.98. The method of claim 90, wherein the gas has a subatmospheric pressure in said interior volume.99. The method of claim 90, wherein the gas has a pressure in said interior volume in a range of from about 20 to about 750 torr.100. The method of claim 90, wherein the vessel comprises a material of construction selected from the group consisting of metals, glasses, ceramics, vitreous materials, polymers, and composite materials.101. The method of claim 100, wherein the vessel comprises a metal material of construction.102. The method of claim 101, wherein said metal is selected from the group consisting of steel, stainless steel, aluminum, copper, brass, bronze, and alloys thereof.103. The method of claim 90, wherein the adsorbent has at least 20% of its porosity in pores with a diameter of less than 2 nanometers.104. The method of claim 90, wherein the fluid comprises boron trifluoride.105. The method of claim 90, wherein the vessel has a rectangular parallelepiped shape.106. The method of claim 90, wherein the vessel has an elongate shape with a square cross-section.107. The method of claim 90, wherein the vessel has a cylindrical shape.108. The method of claim 90, wherein the vessel is of a vertically upstanding configuration.
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