초록 ▼

This invention relates to a liquid phase reagent dispensing apparatus having a diptube and also a metal seal aligned and in contact with the hardened opposing flat surfaces of a top wall member and a protuberance on a side wall member, wherein the hardened opposing flat surfaces of the top wall memb

This invention relates to a liquid phase reagent dispensing apparatus having a diptube and also a metal seal aligned and in contact with the hardened opposing flat surfaces of a top wall member and a protuberance on a side wall member, wherein the hardened opposing flat surfaces of the top wall member and the protuberance have a hardness greater than the hardness of the metal seal. The apparatus further has a temperature sensor and a source chemical level sensor extending through a centrally located portion of the top wall member and generally vertically downwardly to a sump cavity centrally located on a bottom wall member. The dispensing apparatus may be used for dispensing of reagents such as precursors for deposition of materials in the manufacture of semiconductor materials and devices.

대표청구항 ▼

1. A liquid phase reagent dispensing apparatus comprising: a vessel which comprises a removable top wall member, a sidewall member and a bottom wall member configured to form an internal vessel compartment to hold a source chemical up to a fill level and to additionally define an inner gas volume ab

1. A liquid phase reagent dispensing apparatus comprising: a vessel which comprises a removable top wall member, a sidewall member and a bottom wall member configured to form an internal vessel compartment to hold a source chemical up to a fill level and to additionally define an inner gas volume above the fill level;said sidewall member having a protuberance that extends into the internal vessel compartment adjacent to the top wall member;said top wall member and said sidewall member having opposing flat surfaces, wherein the opposing flat surfaces are optionally in contact with one another;fastening means for securing said top wall member to said sidewall member through the opposing flat surfaces that are optionally in contact with one another;said top wall member and said protuberance having opposing flat surfaces, wherein the opposing flat surfaces are not in contact with one another and at least a portion of the opposing flat surfaces are hardened;a metal seal aligned and in contact with the hardened opposing flat surfaces of said top wall member and said protuberance;said bottom wall member having a main floor surface containing a sump cavity therein extending downwardly from the main floor surface, the sump cavity being bounded at its lower end by a sub-floor surface, with at least a portion of the sump cavity being centrally located on the bottom wall member and at least a portion of the sump cavity being non-centrally located on the bottom wall member;a temperature sensor extending from an upper end exterior of the vessel through a centrally located portion of the top wall member and generally vertically downwardly through the inner gas volume into the source chemical to a lower end of that portion of the sump cavity centrally located on the bottom wall member, with the lower end of the temperature sensor being located in non-interfering proximity to the sub-floor surface of the sump cavity;a source chemical level sensor extending from an upper end exterior of the vessel through a non-centrally located portion of the top wall member and generally vertically downwardly through the inner gas volume into the source chemical to a lower end of that portion of the sump cavity non-centrally located on the bottom wall member, with the lower end of the source chemical level sensor being located in non-interfering proximity to the sub-floor surface of the sump cavity;the temperature sensor being operatively arranged in the sump cavity to determine the temperature of source chemical in the vessel, the source chemical level sensor being operatively arranged in the sump cavity to determine the level of source chemical in the vessel, the temperature sensor and source chemical level sensor being located in non-interfering proximity to each other in the sump cavity, with the lower end of the temperature sensor being located at the same or closer proximity to the sub-floor surface of the sump cavity in relation to the lower end of the source chemical level sensor, and the temperature sensor and source chemical level sensor being in source chemical flow communication in the sump cavity;a non-centrally located portion of the top wall member having an inert gas feed inlet opening through which said inert gas can be fed into the inner gas volume above the fill level to pressurize the inner gas volume above the fill level; anda non-centrally located portion of the top wall member having a liquid phase reagent outlet opening comprising a diptube that extends through the inner gas volume into the source chemical and through which liquid phase reagent can be dispensed from said apparatus, said diptube having an outlet end adjacent to the top wall member and an inlet end adjacent to the bottom wall member;wherein said hardened opposing flat surfaces of said top wall member and said protuberance have a hardness greater than the hardness of said metal seal. 2. The liquid phase reagent dispensing apparatus of claim 1 wherein the metal seal comprises an outer metal jacket, an inner elastomeric material or spring, and optionally a liner positioned between said outer metal jacket and said inner elastomeric material or spring. 3. The liquid phase reagent dispensing apparatus of claim 2 wherein the outer metal jacket includes a projection which is annularly formed at a top exterior surface and which abuts against the hardened flat surface of the top wall member, and a projection which is annularly formed at a bottom exterior surface and which abuts against the hardened flat surface of the protuberance. 4. The liquid phase reagent dispensing apparatus of claim 1 wherein the metal seal comprises an annular shaped seal having a cross section provided with an outer circumferential opening and formed in a laterally C-shape or U-shape. 5. The liquid phase reagent dispensing apparatus of claim 1 wherein the hardened opposing flat surfaces of the top wall member and the protuberance are formed by burnishing said opposing flat surfaces. 6. The liquid phase reagent dispensing apparatus of claim 1 wherein the hardened opposing flat surfaces of the top wall member and the protuberance are formed by incorporating a hardening material into the opposing flat surfaces. 7. The liquid phase reagent dispensing apparatus of claim 6 wherein the hardening material comprises Stellite. 8. The liquid phase reagent dispensing apparatus of claim 1 wherein the vessel is made of stainless steel and the outer metal jacket is made of stainless steel. 9. The liquid phase reagent dispensing apparatus of claim 1 having a helium leak rate (unfilled container testing procedure) of less than 9×10−9 standard cubic centimeters per second. 10. The liquid phase reagent dispensing apparatus of claim 1 further comprising: an inert gas feed line extending from the inert gas feed inlet opening upwardly and exteriorly from the top wall member for delivery of inert gas into said inner gas volume above the fill level, the inert gas feed line containing an inert gas flow control valve therein for control of flow of the inert gas therethrough; anda liquid phase reagent discharge line extending from the liquid phase reagent outlet opening upwardly and exteriorly from the top wall member for removal of liquid phase reagent from said vessel, the liquid phase reagent discharge line containing a liquid phase reagent flow control valve therein for control of flow of the liquid phase reagent therethrough. 11. The liquid phase reagent dispensing apparatus of claim 10 further comprising the liquid phase reagent discharge line in liquid phase reagent flow communication with a vaporization apparatus, said vaporization apparatus in vapor phase reagent flow communication with a vapor phase delivery deposition system, said deposition system selected from a chemical vapor deposition system and an atomic layer deposition system. 12. The liquid phase reagent dispensing apparatus of claim 10 further comprising an inert gas source coupled to the inert gas feed line. 13. The liquid phase reagent dispensing apparatus of claim 10 further comprising: a deposition chamber selected from a chemical vapor deposition chamber and an atomic layer deposition chamber;the liquid phase reagent discharge line connecting the liquid phase reagent dispensing apparatus to a vaporization apparatus;a portion of the vaporization apparatus having a carrier gas feed inlet opening through which carrier gas can be fed into said vaporization apparatus to cause vapor of said liquid phase reagent to become entrained in said carrier gas to produce vapor phase reagent;a portion of the vaporization apparatus having a vapor phase reagent outlet opening through which said vapor phase reagent can be dispensed from said vaporization apparatus;a carrier gas feed line extending from the carrier gas feed inlet opening upwardly and exteriorly from the vaporization apparatus for delivery of carrier gas into said vaporization apparatus, the carrier gas feed line containing a carrier gas flow control valve therein for control of flow of the carrier gas therethrough;a vapor phase reagent discharge line extending from the vapor phase reagent outlet opening upwardly and exteriorly from the vaporization apparatus for removal of vapor phase reagent from said vaporization apparatus to said deposition chamber, the vapor phase reagent discharge line containing a vapor phase reagent flow control valve therein for control of flow of the vapor phase reagent therethrough;a heatable susceptor contained within the deposition chamber and located in a receiving relationship to the vaporization apparatus; andan effluent discharge line connected to the deposition chamber; such that vapor phase reagent passes through the vapor phase reagent discharge line and into the deposition chamber, for contact with a substrate on the heatable susceptor and any remaining effluent is discharged through the effluent discharge line. 14. The liquid phase reagent dispensing apparatus of claim 13 wherein said substrate is comprised of a material selected from a metal, a metal silicide, a semiconductor, an insulator and a barrier material. 15. The liquid phase reagent dispensing apparatus of claim 13 wherein said substrate is a patterned wafer. 16. The liquid phase reagent dispensing apparatus of claim 1 wherein the sump cavity comprises a minor fraction of the area of the bottom wall member. 17. The liquid phase reagent dispensing apparatus of claim 1 wherein the sump cavity is defined at least in part by a sloping wall surface. 18. The liquid phase reagent dispensing apparatus of claim 1 wherein the sump cavity has two or three intersecting circular depressions in top plan view of the bottom wall member surface. 19. The liquid phase reagent dispensing apparatus of claim 1 wherein the sump cavity comprises two or three transversely spaced-apart circular depressions in source chemical flow communication with one another, with one of the circular depressions having the lower end of the temperature sensor disposed therein and another of the circular depressions having the lower end of the source chemical level sensor disposed therein. 20. The liquid phase reagent dispensing apparatus of claim 1 wherein the lower end of the source chemical level sensor is in sufficiently close proximity to the sub-floor surface of the sump cavity to permit utilization of at least 95% of source chemical when source chemical is contained in the vessel. 21. The liquid phase reagent dispensing apparatus of claim 1 wherein said source chemical level sensor is selected from the group consisting of ultrasonic sensors, optical sensors, capacitive sensors and float-type sensors, and said temperature sensor comprises a thermowell and thermocouple. 22. The liquid phase reagent dispensing apparatus of claim 1 wherein the vessel comprises a cylindrically shaped side wall member or side wall members defining a non-cylindrical shape. 23. The liquid phase reagent dispensing apparatus of claim 1 wherein the source chemical comprises a liquid or solid material. 24. The liquid phase reagent dispensing apparatus of claim 1 wherein the source chemical comprises a precursor for a metal selected from ruthenium, hafnium, tantalum, molybdenum, platinum, gold, titanium, lead, palladium, zirconium, bismuth, strontium, barium, calcium, antimony and thallium, or a precursor for a metalloid selected from silicon and germanium. 25. The liquid phase reagent dispensing apparatus of claim 1 wherein the vapor or liquid phase reagent comprises a precursor for a metal selected from ruthenium, hafnium, tantalum, molybdenum, platinum, gold, titanium, lead, palladium, zirconium, bismuth, strontium, barium, calcium, antimony and thallium, or a precursor for a metalloid selected from silicon and germanium. 26. A method for delivery of a vapor phase reagent to a deposition chamber comprising: (a) providing a liquid phase reagent dispensing apparatus comprising:a vessel which comprises a removable top wall member, a sidewall member and a bottom wall member configured to form an internal vessel compartment to hold a source chemical up to a fill level and to additionally define an inner gas volume above the fill level;said sidewall member having a protuberance that extends into the internal vessel compartment adjacent to the top wall member;said top wall member and said sidewall member having opposing flat surfaces, wherein the opposing flat surfaces are optionally in contact with one another;fastening means for securing said top wall member to said sidewall member through the opposing flat surfaces that are optionally in contact with one another;said top wall member and said protuberance having opposing flat surfaces, wherein the opposing flat surfaces are not in contact with one another and at least a portion of the opposing flat surfaces are hardened;a metal seal aligned and in contact with the hardened opposing flat surfaces of said top wall member and said protuberance;said bottom wall member having a main floor surface containing a sump cavity therein extending downwardly from the main floor surface, the sump cavity being bounded at its lower end by a sub-floor surface, with at least a portion of the sump cavity being centrally located on the bottom wall member and at least a portion of the sump cavity being non-centrally located on the bottom wall member;a temperature sensor extending from an upper end exterior of the vessel through a centrally located portion of the top wall member and generally vertically downwardly through the inner gas volume into the source chemical to a lower end of that portion of the sump cavity centrally located on the bottom wall member, with the lower end of the temperature sensor being located in non-interfering proximity to the sub-floor surface of the sump cavity;a source chemical level sensor extending from an upper end exterior of the vessel through a non-centrally located portion of the top wall member and generally vertically downwardly through the inner gas volume into the source chemical to a lower end of that portion of the sump cavity non-centrally located on the bottom wall member, with the lower end of the source chemical level sensor being located in non-interfering proximity to the sub-floor surface of the sump cavity;the temperature sensor being operatively arranged in the sump cavity to determine the temperature of source chemical in the vessel, the source chemical level sensor being operatively arranged in the sump cavity to determine the level of source chemical in the vessel, the temperature sensor and source chemical level sensor being located in non-interfering proximity to each other in the sump cavity, with the lower end of the temperature sensor being located at the same or closer proximity to the sub-floor surface of the sump cavity in relation to the lower end of the source chemical level sensor, and the temperature sensor and source chemical level sensor being in source chemical flow communication in the sump cavity;a non-centrally located portion of the top wall member having an inert gas feed inlet opening through which said inert gas can be fed into the inner gas volume above the fill level to pressurize the inner gas volume above the fill level;an inert gas feed line extending from the inert gas feed inlet opening upwardly and exteriorly from the top wall member for delivery of inert gas into said inner gas volume above the fill level, the inert gas feed line containing an inert gas flow control valve therein for control of flow of the inert gas therethrough;a non-centrally located portion of the top wall member having a liquid phase reagent outlet opening comprising a diptube that extends through the inner gas volume into the source chemical and through which liquid phase reagent can be dispensed from said apparatus, said diptube having an outlet end adjacent to the top wall member and an inlet end adjacent to the bottom wall member; anda liquid phase reagent discharge line extending from the liquid phase reagent outlet opening upwardly and exteriorly from the top wall member for removal of liquid phase reagent from said vessel, the liquid phase reagent discharge line containing a liquid phase reagent flow control valve therein for control of flow of the liquid phase reagent therethrough;wherein said hardened opposing flat surfaces of said top wall member and said protuberance have a hardness greater than the hardness of said metal seal;(b) adding liquid phase reagent at ambient temperature to said liquid phase reagent dispensing apparatus;(c) optionally heating a solid source chemical in said liquid phase reagent dispensing apparatus to a temperature sufficient to melt the solid source chemical to provide liquid phase reagent;(d) feeding an inert gas into said liquid phase reagent dispensing apparatus through said inert gas feed line;(e) withdrawing the liquid phase reagent from said liquid phase reagent dispensing apparatus through said diptube and said liquid phase reagent discharge line;(f) providing a vaporization apparatus comprising:a vessel which comprises a top wall member, a sidewall member and a bottom wall member configured to form an internal vessel compartment to vaporize the liquid phase reagent;said liquid phase reagent discharge line connecting the liquid phase reagent dispensing apparatus to said vaporization apparatus;a portion of the vaporization apparatus having a carrier gas feed inlet opening through which carrier gas can be fed into said vaporization apparatus to cause vapor of said liquid phase reagent to become entrained in said carrier gas to produce vapor phase reagent;a portion of the vaporization apparatus having a vapor phase reagent outlet opening through which said vapor phase reagent can be dispensed from said vaporization apparatus;a carrier gas feed line extending from the carrier gas feed inlet opening upwardly and exteriorly from the vaporization apparatus for delivery of carrier gas into said vaporization apparatus, the carrier gas feed line containing a carrier gas flow control valve therein for control of flow of the carrier gas therethrough;a vapor phase reagent discharge line extending from the vapor phase reagent outlet opening upwardly and exteriorly from the vaporization apparatus for removal of vapor phase reagent from said vaporization apparatus to said deposition chamber, the vapor phase reagent discharge line containing a vapor phase reagent flow control valve therein for control of flow of the vapor phase reagent therethrough;(g) feeding the liquid phase reagent into said vaporization apparatus;(h) heating the liquid phase reagent in said vaporization apparatus to a temperature sufficient to vaporize the liquid phase reagent to provide said vapor phase reagent;(i) feeding a carrier gas into said vaporization apparatus through said carrier gas feed line;(j) withdrawing the vapor phase reagent and carrier gas from said vaporization apparatus through said vapor phase reagent discharge line; and(k) feeding the vapor phase reagent and carrier gas into said deposition chamber. 27. The method of claim 26 further comprising: (l) contacting the vapor phase reagent with a substrate on a heatable susceptor within the deposition chamber; and(m) discharging any remaining effluent through an effluent discharge line connected to the deposition chamber. 28. The method of claim 27 wherein said substrate is comprised of a material selected from a metal, a metal silicide, a semiconductor, an insulator and a barrier material. 29. The method of claim 27 wherein said substrate is a patterned wafer. 30. The method of claim 26 in which the deposition chamber is selected from a chemical vapor deposition chamber and an atomic layer deposition chamber.