PVDF pyrolyzate adsorbent and gas storage and dispensing system utilizing same

Patent metadata

Field	Value
Publication number	US-9234628-B2
Application number	US-201414224536-A
Country	US
Kind code	B2
Filing date	Mar 25, 2014
Priority date	Jan 19, 2011
Publication date	Jan 12, 2016
Grant date	Jan 12, 2016

Abstract

A polyvinylidene fluoride (PVDF) pyrolyzate adsorbent is described, having utility for storing gases in an adsorbed state, and from which adsorbed gas may be desorbed to supply same for use. The PVDF pyrolyzate adsorbent can be of monolithic unitary form, or in a bead, powder, film, particulate or other finely divided form. The adsorbent is particularly suited for storage and supply of fluorine-containing gases, such as fluorine gas, nitrogen trifluoride, carbo-fluoride gases, and the like. The adsorbent may be utilized in a gas storage and dispensing system, in which the adsorbent is contained in a supply vessel, from which sorbate gas can be selectively dispensed.

First claim

What is claimed is:

1. A fluid storage and dispensing apparatus, comprising:
a fluid storage and dispensing vessel, holding a fluid storage and dispensing medium comprising a polyvinylidene fluoride pyrolyzate carbon adsorbent in a monolithic or particulate form, adapted for fluid to be reversibly adsorbed thereon,
wherein the vessel is configured to store adsorbed fluid on the polyvinylidene fluoride pyrolyzate carbon adsorbent, and to discharge fluid desorbed from the polyvinylidene fluoride pyrolyzate carbon adsorbent under dispensing conditions.

2. The fluid storage and dispensing apparatus of claim 1 , further comprising a fluid reversibly adsorbed on the polyvinylidene fluoride pyrolyzate carbon adsorbent.

3. The fluid storage and dispensing apparatus of claim 2 , wherein the fluid comprises one or more of arsine, phosphine, boron trichloride, boron trifluoride, silane, germane, phosgene, diborane, ammonia, stibine, hydrogen sulfide, hydrogen selenide, hydrogen telluride, nitrous oxide, hydrogen cyanide, ethylene oxide, deuterated hydrides, halide (chlorine, bromine, fluorine, and iodine) compounds, organometallic compounds, nitrogen trifluoride, fluorine, hydrogen fluoride, diboron tetrafluoride, and carbofluoride compounds.

4. A fluid storage and dispensing apparatus, comprising:
a fluid storage and dispensing vessel, holding a fluid storage and dispensing medium comprising a polyvinylidene fluoride pyrolyzate carbon adsorbent adapted for fluid to be reversibly adsorbed thereon,
wherein the vessel is configured to store adsorbed fluid on the polyvinylidene fluoride pyrolyzate carbon adsorbent, and to discharge fluid desorbed from the polyvinylidene fluoride pyrolyzate carbon adsorbent under dispensing conditions,
further comprising a fluid reversibly adsorbed on the polyvinylidene fluoride pyrolyzate carbon adsorbent,
wherein the fluid comprises a fluorine-containing fluid.

5. The fluid storage and dispensing apparatus of claim 4 , wherein the fluorine-containing fluid comprises fluorine gas.

6. The fluid storage and dispensing apparatus of claim 4 , wherein the fluorine-containing fluid comprises NF 3 .

7. The fluid storage and dispensing apparatus of claim 1 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent is of monolithic form.

8. The fluid storage and dispensing apparatus of claim 1 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent is of particulate form.

9. The fluid storage and dispensing apparatus of claim 1 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent comprises porosity including pores of a size in a range of from 0.2 to 5 nanometers.

10. The fluid storage and dispensing apparatus of claim 9 , having porosity, wherein at least 30% of the porosity of the polyvinylidene fluoride pyrolyzate carbon adsorbent comprises pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 50% of the porosity comprises pores of diameter <2 nanometers.

11. The fluid storage and dispensing apparatus of claim 1 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent has a bulk density in a range of from 0.6 to 1.8 grams per cubic centimeter.

12. The fluid storage and dispensing apparatus of claim 1 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent has a fluorine gas permeability in a range of from 100 to 600 cc/psi/cm 2 /min at 275 kPa pressure.

13. The fluid storage and dispensing apparatus of claim 1 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent is in the form of discs that are vertically stacked in the fluid storage and dispensing vessel to form a stacked array in which successive discs are in face-to-face abutting relationship to one another.

14. The fluid storage and dispensing apparatus of claim 13 , wherein the polyvinylidene fluoride pyrolyzate carbon adsorbent has a bulk density in a range of from 0.6 to 1.8 grams per cubic centimeter, a fluorine gas permeability in a range of from 100 to 600 cc/psi/cm 2 /min at 275 kPa pressure, and porosity including pores of a size in a range of from 0.2 to 5 nanometers, wherein at least 30% of the porosity of the polyvinylidene fluoride pyrolyzate carbon adsorbent comprises pores having a size in a range of from about 0.3 to about 0.72 nanometer, and at least 50% of the porosity comprises pores of diameter <2 nanometers.

15. A method of supplying fluid for use in manufacturing, comprising charging an adsorbable fluid to a fluid storage and dispensing apparatus according to claim 1 , for adsorption of the adsorbable fluid on the polyvinylidene fluoride pyrolyzate carbon adsorbent.

16. The method of claim 15 , wherein said charging is carried out in a fill operation wherein pressure of the adsorbable fluid is monitored during the fill operation.

17. A manufacturing facility comprising a fluid storage and dispensing apparatus according to claim 2 , coupled to flow circuitry for delivering fluid discharged from the fluid storage and dispensing vessel under dispensing conditions to a fluid-utilizing apparatus.

18. A manufacturing facility comprising a fluid storage and dispensing apparatus, comprising:
a fluid storage and dispensing vessel, holding a fluid storage and dispensing medium comprising a polyvinylidene fluoride pyrolyzate carbon adsorbent adapted for fluid to be reversibly adsorbed thereon,
wherein the vessel is configured to store adsorbed fluid on the polyvinylidene fluoride pyrolyzate carbon adsorbent, and to discharge fluid desorbed from the polyvinylidene fluoride pyrolyzate carbon adsorbent under dispensing conditions,
further comprising a fluid reversibly adsorbed on the polyvinylidene fluoride pyrolyzate carbon adsorbent,
wherein the fluid storage and dispensing apparatus is coupled to flow circuitry for delivering fluid discharged from the fluid storage and dispensing vessel under dispensing conditions to a fluid-utilizing apparatus,
wherein the fluid reversibly adsorbed on the polyvinylidene fluoride pyrolyzate carbon adsorbent comprises fluorine gas or nitrogen fluoride gas, the fluid-utilizing apparatus comprises a semiconductor manufacturing apparatus, and the fluid storage and dispensing apparatus is configured to flow the fluid to the semiconductor manufacturing apparatus for cleaning thereof.

19. The manufacturing facility of claim 18 , wherein the semiconductor manufacturing apparatus comprises a vapor deposition chamber or an ion implant chamber.

20. A method of manufacturing a semiconductor, flat-panel display, or solar product, comprising supplying gas for said manufacturing from a fluid storage and dispensing apparatus according to claim 1 .

Assignees

• Entegris Inc

Inventors

• Wilson Shaun M
• Sturm Edward A

Classifications

• F17C11/00 Primary

  Use of gas-solvents or gas-sorbents in vessels {(absorbing compositions for acetylene C10L3/04; absorbing compositions for hydrogen C01B3/0005)} · CPC title

• C23C16/4405

  Cleaning of reactor or parts inside the reactor by using reactive gases · CPC title

• B01J20/28083

  being in the range 2-50 nm, i.e. mesopores · CPC title

• B01J20/2808

  being less than 2 nm, i.e. micropores or nanopores · CPC title

• B01J20/20 Primary

  comprising free carbon; comprising carbon obtained by carbonising processes · CPC title