US20140013778A1 - Thermal insulation technique for ultra low temperature cryogenic processor - Google Patents

Thermal insulation technique for ultra low temperature cryogenic processor Download PDF

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Publication number
US20140013778A1
US20140013778A1 US13/731,013 US201213731013A US2014013778A1 US 20140013778 A1 US20140013778 A1 US 20140013778A1 US 201213731013 A US201213731013 A US 201213731013A US 2014013778 A1 US2014013778 A1 US 2014013778A1
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Prior art keywords
tubings
heat exchanger
cryogenic
vacuum
vacuum region
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Abandoned
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US13/731,013
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John Dain
Boyd Bowdish
Nick Henneman
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Reflect Scientific Inc
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Reflect Scientific Inc
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Priority claimed from US11/934,696 external-priority patent/US7823394B2/en
Application filed by Reflect Scientific Inc filed Critical Reflect Scientific Inc
Priority to US13/731,013 priority Critical patent/US20140013778A1/en
Publication of US20140013778A1 publication Critical patent/US20140013778A1/en
Abandoned legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J10/00Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17CVESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C13/00Details of vessels or of the filling or discharging of vessels
    • F17C13/001Thermal insulation specially adapted for cryogenic vessels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002Nozzle-type elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00108Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00162Controlling or regulating processes controlling the pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00186Controlling or regulating processes controlling the composition of the reactive mixture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00193Sensing a parameter
    • B01J2219/00195Sensing a parameter of the reaction system
    • B01J2219/002Sensing a parameter of the reaction system inside the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00222Control algorithm taking actions
    • B01J2219/00227Control algorithm taking actions modifying the operating conditions
    • B01J2219/00229Control algorithm taking actions modifying the operating conditions of the reaction system
    • B01J2219/00231Control algorithm taking actions modifying the operating conditions of the reaction system at the reactor inlet

Definitions

  • This invention relates to a thermal insulation technique for ultra low temperature cryogenic processors.
  • Vacuum insulating panels are used conventionally for thermal insulation.
  • Known vacuum insulating panels consist of a pre-compressed porous filling, a porous pressboard or an open-cell rigid foam as substrate, which is enveloped by a gas-tight film, wherein the film is heat-seated or bonded after the evacuation.
  • vacuum insulating panels precipitated and dried silicas, silica gels, fly ash, open-cell foams on an organic base such as open-cell rigid polyurethane foams or bonded rigid polyurethane foam paste.
  • Vacuum insulating panels of this type are used in the manufacture of cold rooms, e.g., refrigerators or refrigerated containers, with the latter being inserted between the outer and inner casing and the gap left between the outer and inner casing being filled with foam.
  • U.S. Pat. No. 6,164,030 discloses an apparatus which consists of a rigid plate and a vacuum insulation panel, in which the vacuum insulation panel is fixed to the rigid plate by a polyurethane foam applied as a liquid reaction mixture, wherein the vacuum insulation panel contains open-cell rigid plastics foam and/or open-cell rigid plastics foam recyclate.
  • systems and methods are disclosed to provide a cryogenic processor apparatus with an outer housing; an inner housing coupled to the external housing to define a vacuum region there between; and material disposed in the vacuum region to provide redundant insulation and structural support at a cryogenic temperature.
  • the apparatus includes an external housing with flat sides; an inner housing coupled to the external housing to define a vacuum region there between; material disposed in the vacuum region to provide redundant insulation and structural support; and a cryogenic heat exchanger contained in the inner housing.
  • ULT ultra low temperature
  • the material can be an insulation material with one of: a silica micro balloon, polyisocyanurate.
  • the vacuum region can be processed by removing residual water vapor and other partial pressure of contaminants.
  • the vacuum region is evacuated to a partial pressure of approximately 0.2 milliTorr.
  • the cryogenic heat exchanger can include one or more tubings and may include redundant tubings.
  • the cryogenic heat exchanger can be U-shaped tubings covering at least three walls of the payload bay.
  • the cryogenic heat exchanger can include tubings covering at least four sides of the payload bay.
  • the cryogenic heat exchanger can be one or more coils positioned on the top and/or the bottom of the vessel.
  • a port can connect to the one or more tubings to provide input and output connections thereto.
  • a door can allow access to the payload bay, wherein the door comprises three or more materials having different thermal characteristics.
  • a method to provide ultra low temperature processing and/or storage includes providing insulation and structural support using a material disposed in a vacuum region between an external housing and an inner housing; and cryogenically processing one or more compartments contained in the payload bay.
  • the material can be an insulation material with silica micro balloon technology.
  • the process can remove water vapor, partial pressure contaminates and atmospheric gases from the vacuum region.
  • the process includes evacuating the vacuum region to approximately 0.2 millitorr.
  • the cryogenic heat exchanger can have one or more heat exchange tubings, and can include redundant tubings.
  • the redundant tubings can be a complete set of heat exchange tubings operating in parallel with the primary heat exchange tubings.
  • the redundant tubings can have one or more tubings branched from the primary heat exchange tubings.
  • the cryogenic heat exchanger can also include U-shaped tubings covering at least three walls of the inner housing.
  • the tubings can cover at least four sides of the inner housing.
  • a door can be formed with a plurality of materials each having different thermal characteristics.
  • a changeable rack assembly is supported in the chamber.
  • the system can transmit energy from the payload bay into the heat exchanger through the changeable rack assembly.
  • a negative pressure in the payload bay can be maintained through the use of pneumatic seals on the main door assembly.
  • the cryogenics vacuum pumping via the heat exchanger can provide energy removal from the payload bay and into the heat exchanger.
  • the surfaces of at least one of the external and inner housing can be flat surfaces.
  • a method to insulate a vessel includes placing a plurality of shells on all sides of the vessel without providing a direct energy pathway from outer walls of the vessel to the inner walls of the vessel; placing the shells under a vacuum; cryogenically cooling the shells to a cryogenic temperature; and while under vacuum, allowing the shell temperature to rise from the cryogenic temperature to ambient temperature.
  • the process can include milling spaced-apart pathways in the shells. Such millings facilitate an evacuation of the trapped spaces of the shells and allowing for a desorbtion of a surface area of the shells.
  • a vacuum pump can maintain a partial pressure of the vacuum in the vessel to below approximately 10 millitorr.
  • the vacuum pump is a non-oil based pump. Initially, the process evacuates the shells to a total pressure of approximately 500 millitorr. The process then cryogenically cools the shells to a temperature of less than approximately ⁇ 175° C. Next, gettered gases can be removed by a pseudo thermo/kinetic energy transfer during the rise to ambient temperature.
  • the shells can be a foam material.
  • the shell layout prevents heat gain energy from migrating from the outer walls to the inner walls by presenting at least two 90 degree flow pathway changes.
  • an insulated vessel in another aspect, includes outer walls; inner walls spaced apart from the outer walls to define a vacuumed insulation volume; and a plurality of shells placed in the insulation volume without providing a direct energy pathway from outer walls of the vessel to the inner walls of the vessel, wherein the shells are cryogenically cooled to a cryogenic temperature and while under vacuum, the shell temperature is raised from the cryogenic temperature to ambient temperature.
  • Implementations of the above aspect may include one or more of the following.
  • Spaced-apart pathways can be milled in the shells. The pathways facilitate an evacuation of the trapped spaces of the shells and allowing for a desorbtion of a surface area of the shells.
  • a vacuum pump can maintain a partial pressure of the vacuum in the insulation volume to below approximately 10 millitorr.
  • the vacuum can be provided using a non-oil based pump.
  • the pump can initially evacuate the insulation volume to a total pressure of approximately 500 millitorr.
  • a cryogenic heat exchanger can cryogenically cool the shells to a temperature below approximately ⁇ 175° C. Gettered gases can be removed by a pseudo thermo/kinetic energy transfer during the rise to ambient temperature.
  • Each shell can be a foam material. The shells prevent heat gain energy from migrating from the outer walls to the inner walls by presenting at least two 90 degree flow pathway changes.
  • the system has a thermal insulation technique that combines a highly non-compressible foam and traditional vacuum processing techniques to produce a novel insulation technique.
  • This technique can be used to reduce the heat gain properties of a low temperature vessels and allow for the manufacture of square, flat walled vacuum chambers that demonstrate no structural deformation or metal fatigue during the evacuation process.
  • the theoretical R-value of this technique is greater then 100 as measured by the International System of Units—RSI.
  • FIG. 1 shows an exemplary process to insulate a vessel.
  • FIG. 2 shows an exemplary shell arrangement
  • FIG. 3 shows an assembly of the vessel with outer walls, shells, and the payload chamber.
  • FIG. 4 shows an exemplary payload chamber enclosed by the shell.
  • FIG. 5 shows an exemplary cold vacuum processing operation.
  • FIG. 1 shows an exemplary process to insulate a vessel such as a biological storage chamber, among others.
  • the process forms a plurality of foam shells on all sides of a vessel without a direct energy pathway from outer walls of the vessel to the inner walls of the vessel ( 1 ).
  • the process places the foam shells under vacuum ( 2 ).
  • the process then cryogenically cools the foam shells ( 3 ); and while under vacuum, allowing the foam shell temperature to rise from a cryogenic temperature to an ambient temperature ( 4 ).
  • FIG. 2 shows an exemplary shell arrangement.
  • the shell can be made of foam, among other materials.
  • two outside back shell portions 25 and 26 are positioned adjacent each other. Portions 25 in turn faces inner back shell portions 27 and 33 . These portions in turn are surrounded on left and right sides by a pair of side shell assembly having an outside side shell portions 28 and 29 that face inside side shell portions 30 and 31 .
  • the back shell portions and the side shell portions are in turn connected to top and bottom shell assemblies.
  • the bottom shell assembly includes outer bottom shelf portions 19 and 34 facing inner bottom shelf portions 20 - 21 .
  • the top shell assembly includes outer top shelf portions 22 and 32 that face inner top shelf portions 23 - 24 .
  • the top shell assembly include openings 22 that allow cryogenic coolants to enter and exit a payload chamber as shown in more details below.
  • each foam piece is four inches thick and is made from a polyisocyanurate material.
  • the vacuum vessel is made of austenitic stainless steel, type 302 , 304 , 316 , 321 or 347 .
  • the foam design places foam sections on all sides of a vessel and will be designed so that there are no direct energy pathways from the outer walls to the inner wall.
  • the arrangement challenges any heat gain energy from migrating from the outer wall to the cryogenically tempered inner surface by presenting at least two 90 degree flow pathway changes. All energy migrating from outer to inner is gettered by the kinetic properties of the foam, while in molecular flow regime.
  • All foam sections will have vacuum pathways milled into them which are 0.065′′ in cross section, spaced in an arrangement that facilitates the evacuation of the trapped spaces of the foam sections and allowing for the desorbtion of the surface area of the foam to a minimum of 100 monolayers in one embodiment.
  • the foam After the milling operation, the foam itself has enough surface area and flow obstructions as to prevent serious back flow of contaminates into the vacuum space.
  • Vacuum channels are placed on the foam to allow for two processes to happen. First, the channels facilitate the general evacuation of the chambers and second, the channels facilitate the desorbtion of water vapor from the foam surface.
  • the vacuum processing reduces the partial pressure of the vacuum vessel to a point lower than 10 millitorr as measured by a thermocouple or similar total pressure gauge.
  • the use of non-oil based vacuum pumps prevents the back streaming of residual water and oil vapor with its contaminating gas load.
  • a cold processing technique is applied to the shells.
  • the technique includes of three separate steps.
  • the assembly is evacuated to a total pressure of approximately 500 millitorr.
  • the specific ultimate pressure is not important.
  • the assembly is then cryogenically cooled to a temperature of no more then ⁇ 175° C. as measured on the inner wall of the vacuum chamber. This getters contaminant gases onto the inner wall of the vacuum chamber via thermodynamic processes, thus conditioning the foam.
  • the vacuum pump system is connected and applied to the vacuum chamber, the temperature is allowed rise to ambient.
  • the vacuum pump removes all of the gettered gases by way of a pseudo thermo/kinetic energy transfer.
  • the foam is a Polyisocyanurate Insulation that has the following specifications:
  • FIG. 3 shows an assembly of a vessel 110 with outer walls, shells, and inner walls formed by the exterior of the payload chamber.
  • FIG. 3 shows the five-sided outer “tub” 110 A assembled with a lining of insulation, into which is inserted metal inner “tub” 124 , typically of 16 gauge stainless steel, having a front flange which extends around the perimeter.
  • metal inner “tub” 124 typically of 16 gauge stainless steel, having a front flange which extends around the perimeter.
  • This is seamlessly laser-welded to the alter tub 110 all around in a no leak manner to form an insulation tub 110 B with the five hollow walls totally enclosed and filled with the shell portions 112 , 122 , 116 , 118 , 120 and 122 .
  • More details on the vessel 110 are disclosed in co-pending application Ser. No. 11/890,451, filed on Aug. 7, 2007, the content of which is incorporated by reference.
  • FIG. 4 shows an exemplary assembled payload chamber enclosed by an insulation volume where the shells are placed.
  • the rigidity and high compressive strength of the shell material serve to counteract and minimize inward bending distortion of the two opposed metal sheets due to stress from the internal vacuum and external atmospheric pressure as the shell material provides sufficient compressive strength.
  • FIG. 5 shows an exemplary cold vacuum processing operation.
  • the vessel is constructed ( 200 ) and a visual inspection is done ( 202 ) in accordance with a manufacturing protocol ( 204 ). If the visual inspection passes, a primary evacuation operation is done ( 206 ). The primary evacuation can be done using a mechanical pump ( 208 ). After the primary evacuation, a pressure reading is done ( 210 ). The reading tests that a total pressure of about 500 millitorr is in the chamber within 60 minutes ( 212 ).
  • the system performs a leak check using an atmospheric helium leak detector ( 222 ). The system confirms that the leak rate is less than 10 e-6 atm-cc/sec in one embodiment ( 223 ).
  • the system is cooled to less than ⁇ 175 degree C. ( 224 ) while a continual vacuum pumping dual stage turbo molecular pump is operated ( 225 ).
  • a pressure reading is taken ( 226 ).
  • the pressure is less than 10 millitorr ( 228 ).
  • the system also checks for leak using the atmospheric helium leak detector ( 230 ).
  • the helium leak rate is ascertained ( 232 ).
  • the temperature of the vessel is then allowed to rise to ambient temperature while under vacuum ( 234 ).
  • a final ultimate pressure evacuation is done ( 236 ) and the vessel is sealed ( 240 ).

Abstract

Systems and methods are disclosed to provide a cryogenic processor apparatus with an outer housing; an inner housing coupled to the external housing to define a vacuum region there between; and material disposed in the vacuum region to provide redundant insulation and structural support at a cryogenic temperature.

Description

  • This application is a continuation of application Ser. No. 11/934,696 filed on Nov. 2, 2007 and 12/984,206, filed Sep. 30, 2010, the content of which is incorporated by reference.
  • BACKGROUND OF THE INVENTION
  • This invention relates to a thermal insulation technique for ultra low temperature cryogenic processors.
  • Vacuum insulating panels are used conventionally for thermal insulation. Known vacuum insulating panels consist of a pre-compressed porous filling, a porous pressboard or an open-cell rigid foam as substrate, which is enveloped by a gas-tight film, wherein the film is heat-seated or bonded after the evacuation.
  • The following, for example, are used as filling materials for vacuum insulating panels: precipitated and dried silicas, silica gels, fly ash, open-cell foams on an organic base such as open-cell rigid polyurethane foams or bonded rigid polyurethane foam paste. Vacuum insulating panels of this type are used in the manufacture of cold rooms, e.g., refrigerators or refrigerated containers, with the latter being inserted between the outer and inner casing and the gap left between the outer and inner casing being filled with foam.
  • The fitting of the vacuum insulation panels into refrigerator casings nevertheless presents problems. According to the current state of the art, they are bonded onto a plate—for example, a metal cassette—by means of a double-sided adhesive film. This combination plate can then be processed further into a sandwich panel, for example, a refrigerator door, wherein the cavity left is conventionally filled with foam.
  • As a result, on the one hand, a complicated, multi-step process is required, and on the other hand, the insulation volume is affected by the foam, which is less efficient in insulation terms when compared with a vacuum insulation panel. Arrangements of this type are also, to only a limited extent, without thermal bridges.
  • U.S. Pat. No. 6,164,030 discloses an apparatus which consists of a rigid plate and a vacuum insulation panel, in which the vacuum insulation panel is fixed to the rigid plate by a polyurethane foam applied as a liquid reaction mixture, wherein the vacuum insulation panel contains open-cell rigid plastics foam and/or open-cell rigid plastics foam recyclate.
  • SUMMARY
  • In a first aspect, systems and methods are disclosed to provide a cryogenic processor apparatus with an outer housing; an inner housing coupled to the external housing to define a vacuum region there between; and material disposed in the vacuum region to provide redundant insulation and structural support at a cryogenic temperature.
  • In another aspect, systems and methods are disclosed to provide an ultra low temperature (ULT) cryogenic processor apparatus. The apparatus includes an external housing with flat sides; an inner housing coupled to the external housing to define a vacuum region there between; material disposed in the vacuum region to provide redundant insulation and structural support; and a cryogenic heat exchanger contained in the inner housing.
  • Implementations of the above aspect may include one or more of the following. The material can be an insulation material with one of: a silica micro balloon, polyisocyanurate. The vacuum region can be processed by removing residual water vapor and other partial pressure of contaminants. The vacuum region is evacuated to a partial pressure of approximately 0.2 milliTorr. The cryogenic heat exchanger can include one or more tubings and may include redundant tubings. The cryogenic heat exchanger can be U-shaped tubings covering at least three walls of the payload bay. The cryogenic heat exchanger can include tubings covering at least four sides of the payload bay. Alternatively, the cryogenic heat exchanger can be one or more coils positioned on the top and/or the bottom of the vessel. A port can connect to the one or more tubings to provide input and output connections thereto. A door can allow access to the payload bay, wherein the door comprises three or more materials having different thermal characteristics.
  • In another aspect, a method to provide ultra low temperature processing and/or storage includes providing insulation and structural support using a material disposed in a vacuum region between an external housing and an inner housing; and cryogenically processing one or more compartments contained in the payload bay.
  • Implementations of the above aspect may include one or more of the following. The material can be an insulation material with silica micro balloon technology. The process can remove water vapor, partial pressure contaminates and atmospheric gases from the vacuum region. The process includes evacuating the vacuum region to approximately 0.2 millitorr. The cryogenic heat exchanger can have one or more heat exchange tubings, and can include redundant tubings. The redundant tubings can be a complete set of heat exchange tubings operating in parallel with the primary heat exchange tubings. The redundant tubings can have one or more tubings branched from the primary heat exchange tubings. The cryogenic heat exchanger can also include U-shaped tubings covering at least three walls of the inner housing. The tubings can cover at least four sides of the inner housing. A door can be formed with a plurality of materials each having different thermal characteristics. A changeable rack assembly is supported in the chamber. The system can transmit energy from the payload bay into the heat exchanger through the changeable rack assembly. A negative pressure in the payload bay can be maintained through the use of pneumatic seals on the main door assembly. The cryogenics vacuum pumping via the heat exchanger can provide energy removal from the payload bay and into the heat exchanger. The surfaces of at least one of the external and inner housing can be flat surfaces.
  • In another aspect, a method to insulate a vessel includes placing a plurality of shells on all sides of the vessel without providing a direct energy pathway from outer walls of the vessel to the inner walls of the vessel; placing the shells under a vacuum; cryogenically cooling the shells to a cryogenic temperature; and while under vacuum, allowing the shell temperature to rise from the cryogenic temperature to ambient temperature.
  • Implementations of the above aspect may include one or more of the following. The process can include milling spaced-apart pathways in the shells. Such millings facilitate an evacuation of the trapped spaces of the shells and allowing for a desorbtion of a surface area of the shells. A vacuum pump can maintain a partial pressure of the vacuum in the vessel to below approximately 10 millitorr. The vacuum pump is a non-oil based pump. Initially, the process evacuates the shells to a total pressure of approximately 500 millitorr. The process then cryogenically cools the shells to a temperature of less than approximately −175° C. Next, gettered gases can be removed by a pseudo thermo/kinetic energy transfer during the rise to ambient temperature. The shells can be a foam material. The shell layout prevents heat gain energy from migrating from the outer walls to the inner walls by presenting at least two 90 degree flow pathway changes.
  • In another aspect, an insulated vessel includes outer walls; inner walls spaced apart from the outer walls to define a vacuumed insulation volume; and a plurality of shells placed in the insulation volume without providing a direct energy pathway from outer walls of the vessel to the inner walls of the vessel, wherein the shells are cryogenically cooled to a cryogenic temperature and while under vacuum, the shell temperature is raised from the cryogenic temperature to ambient temperature.
  • Implementations of the above aspect may include one or more of the following. Spaced-apart pathways can be milled in the shells. The pathways facilitate an evacuation of the trapped spaces of the shells and allowing for a desorbtion of a surface area of the shells. A vacuum pump can maintain a partial pressure of the vacuum in the insulation volume to below approximately 10 millitorr. The vacuum can be provided using a non-oil based pump. The pump can initially evacuate the insulation volume to a total pressure of approximately 500 millitorr. A cryogenic heat exchanger can cryogenically cool the shells to a temperature below approximately −175° C. Gettered gases can be removed by a pseudo thermo/kinetic energy transfer during the rise to ambient temperature. Each shell can be a foam material. The shells prevent heat gain energy from migrating from the outer walls to the inner walls by presenting at least two 90 degree flow pathway changes.
  • Advantages of the preferred embodiment may include one or more of the following. The system has a thermal insulation technique that combines a highly non-compressible foam and traditional vacuum processing techniques to produce a novel insulation technique. This technique can be used to reduce the heat gain properties of a low temperature vessels and allow for the manufacture of square, flat walled vacuum chambers that demonstrate no structural deformation or metal fatigue during the evacuation process. The theoretical R-value of this technique is greater then 100 as measured by the International System of Units—RSI.
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • FIG. 1 shows an exemplary process to insulate a vessel.
  • FIG. 2 shows an exemplary shell arrangement.
  • FIG. 3 shows an assembly of the vessel with outer walls, shells, and the payload chamber.
  • FIG. 4 shows an exemplary payload chamber enclosed by the shell.
  • FIG. 5 shows an exemplary cold vacuum processing operation.
  • DESCRIPTION
  • FIG. 1 shows an exemplary process to insulate a vessel such as a biological storage chamber, among others. The process forms a plurality of foam shells on all sides of a vessel without a direct energy pathway from outer walls of the vessel to the inner walls of the vessel (1). Next, the process places the foam shells under vacuum (2). The process then cryogenically cools the foam shells (3); and while under vacuum, allowing the foam shell temperature to rise from a cryogenic temperature to an ambient temperature (4).
  • FIG. 2 shows an exemplary shell arrangement. The shell can be made of foam, among other materials. In FIG. 2, two outside back shell portions 25 and 26 are positioned adjacent each other. Portions 25 in turn faces inner back shell portions 27 and 33. These portions in turn are surrounded on left and right sides by a pair of side shell assembly having an outside side shell portions 28 and 29 that face inside side shell portions 30 and 31. The back shell portions and the side shell portions are in turn connected to top and bottom shell assemblies. The bottom shell assembly includes outer bottom shelf portions 19 and 34 facing inner bottom shelf portions 20-21. The top shell assembly includes outer top shelf portions 22 and 32 that face inner top shelf portions 23-24. The top shell assembly include openings 22 that allow cryogenic coolants to enter and exit a payload chamber as shown in more details below.
  • In one embodiment, each foam piece is four inches thick and is made from a polyisocyanurate material. The vacuum vessel is made of austenitic stainless steel, type 302, 304, 316, 321 or 347. The foam design places foam sections on all sides of a vessel and will be designed so that there are no direct energy pathways from the outer walls to the inner wall. The arrangement challenges any heat gain energy from migrating from the outer wall to the cryogenically tempered inner surface by presenting at least two 90 degree flow pathway changes. All energy migrating from outer to inner is gettered by the kinetic properties of the foam, while in molecular flow regime. All foam sections will have vacuum pathways milled into them which are 0.065″ in cross section, spaced in an arrangement that facilitates the evacuation of the trapped spaces of the foam sections and allowing for the desorbtion of the surface area of the foam to a minimum of 100 monolayers in one embodiment. After the milling operation, the foam itself has enough surface area and flow obstructions as to prevent serious back flow of contaminates into the vacuum space. Vacuum channels are placed on the foam to allow for two processes to happen. First, the channels facilitate the general evacuation of the chambers and second, the channels facilitate the desorbtion of water vapor from the foam surface. The vacuum processing reduces the partial pressure of the vacuum vessel to a point lower than 10 millitorr as measured by a thermocouple or similar total pressure gauge. The use of non-oil based vacuum pumps prevents the back streaming of residual water and oil vapor with its contaminating gas load.
  • In addition to using oil free vacuum pumps, a cold processing technique is applied to the shells. The technique includes of three separate steps.
  • Firstly, the assembly is evacuated to a total pressure of approximately 500 millitorr. The specific ultimate pressure is not important.
  • Secondly, the assembly is then cryogenically cooled to a temperature of no more then −175° C. as measured on the inner wall of the vacuum chamber. This getters contaminant gases onto the inner wall of the vacuum chamber via thermodynamic processes, thus conditioning the foam.
  • Lastly, while the vacuum pump system is connected and applied to the vacuum chamber, the temperature is allowed rise to ambient. The vacuum pump removes all of the gettered gases by way of a pseudo thermo/kinetic energy transfer.
  • The following examples are intended to explain the invention in greater detail, but without limiting it in its scope. In one exemplary embodiment, the foam is a Polyisocyanurate Insulation that has the following specifications:
      • Compressive Strength 3 D 1621 lb/in2 kPa
      • Parallel to Rise (Thickness) 140 970
      • Perpendicular to Rise (Width) 130 900
      • Perpendicular to Rise (Length) 130 900
      • Compressive Modulus D 1621 lb/in2 kPa
      • Parallel to Rise (Thickness) 3100 21400
      • Perpendicular to Rise (Width) 2800 19300
      • Perpendicular to Rise (Length) 2800 19300
      • Shear Strength C 273 lb/in2 kPa
      • Parallel to Rise 80 550
      • Shear Modulus C 273 lb/in2 kPa
      • Parallel to Rise 800 5500
      • Tensile Strength D 1623 lb/in2 kPa
      • Parallel to Rise (Thickness) 80 550
      • Tensile Modulus D 1623 lb/in2 kPa
      • Parallel to Rise (Thickness) 2800 19300
      • Flexural Strength C 203 lb/in2 kPa
      • Parallel to Rise 160 1100
      • Flexural Modulus C 203 lb/in2 kPa
      • Parallel to Rise 5800 40000
      • k-Factor (75° F. (24° C.) mean temp.) C 518
      • BTU·in/hr·ft2·° F. W/m° C.
      • Initial 0.180 0.026
      • Aged 180 days @ 75° F. (24° C.) 0.200 0.029
      • R-Value/in (75° F. (24° C.) mean temp.) C 518
      • Hr·ft2·° F./BTU m2·° C./W
      • Initial 5.5 0.97
      • Aged 180 days @ 75° F. (24° C.) 5.0 0.88
      • Closed Cell Content D 2856% 97% 97
      • Water Absorption C 272% by Volume 0.7% by Volume 0.7
      • Water Vapor Permeability E 96 Perm-Inch 1.1
      • (ng/Pa·s·m) 1.6
      • Dimensional Stability 4 D 2126
      • @ −40° F. (−40° C.), 7 days
      • Length % Change −0.3% Change −0.3
      • Volume % Change −0.1% Change −0.1
      • @ 158° F. (70° C.)/97% Relative Humidity, 7 days
      • Length % Change 0.4% Change 0.4
      • Volume % Change 0.7% Change 0.7
      • @ −10° F. (−23° C.), 7 days
      • Length % Change −0.2% Change −0.2
      • Volume % Change −0.7% Change −0.7
      • @ 300° F. (149° C.), 7 days
      • Length % Change −0.4% Change −0.4
      • Volume % Change −1% Change −1
      • Service Temperature 5° F. −297 to +300° C. −183 to +149
  • FIG. 3 shows an assembly of a vessel 110 with outer walls, shells, and inner walls formed by the exterior of the payload chamber. FIG. 3 shows the five-sided outer “tub” 110A assembled with a lining of insulation, into which is inserted metal inner “tub” 124, typically of 16 gauge stainless steel, having a front flange which extends around the perimeter. This is seamlessly laser-welded to the alter tub 110 all around in a no leak manner to form an insulation tub 110B with the five hollow walls totally enclosed and filled with the shell portions 112, 122, 116, 118, 120 and 122. More details on the vessel 110 are disclosed in co-pending application Ser. No. 11/890,451, filed on Aug. 7, 2007, the content of which is incorporated by reference.
  • FIG. 4 shows an exemplary assembled payload chamber enclosed by an insulation volume where the shells are placed. In one embodiment, this shell portions can be first purged of moisture at 120 degrees C. then evacuated at 100 degrees C. to a vacuum of approximately 0.0002 torr (i.e. 02 millitorrs, 1 torr=1/760 atmosphere) and then sealed off as a vacuum-insulation-walled enclosure.
  • The rigidity and high compressive strength of the shell material serve to counteract and minimize inward bending distortion of the two opposed metal sheets due to stress from the internal vacuum and external atmospheric pressure as the shell material provides sufficient compressive strength.
  • FIG. 5 shows an exemplary cold vacuum processing operation. First, the vessel is constructed (200) and a visual inspection is done (202) in accordance with a manufacturing protocol (204). If the visual inspection passes, a primary evacuation operation is done (206). The primary evacuation can be done using a mechanical pump (208). After the primary evacuation, a pressure reading is done (210). The reading tests that a total pressure of about 500 millitorr is in the chamber within 60 minutes (212). Next, the system performs a leak check using an atmospheric helium leak detector (222). The system confirms that the leak rate is less than 10 e-6 atm-cc/sec in one embodiment (223). Next, the system is cooled to less than −175 degree C. (224) while a continual vacuum pumping dual stage turbo molecular pump is operated (225). Next, a pressure reading is taken (226). Preferably, the pressure is less than 10 millitorr (228). The system also checks for leak using the atmospheric helium leak detector (230). The helium leak rate is ascertained (232). The temperature of the vessel is then allowed to rise to ambient temperature while under vacuum (234). A final ultimate pressure evacuation is done (236) and the vessel is sealed (240).
  • Although the invention has been described in detail in the foregoing for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention except as it may be limited by the claims.

Claims (23)

What is claimed is:
1) A cryogenic processor apparatus, comprising:
a) an outer housing;
b) an inner housing coupled to the external housing to define a vacuum region there between;
c) material disposed in the vacuum region to provide redundant insulation and structural support at a cryogenic temperature.
2) The apparatus of claim 1, wherein the material comprises an insulation material with one of: a silica micro balloon, polyisocyanurate.
3) The apparatus of claim 1, wherein the vacuum region is processed using a novel method of removing residual water vapor and other partial pressure of contaminants.
4) The apparatus of claim 1, wherein the vacuum region is evacuated to a partial pressure of approximately 0.2 milliTorr.
5) The apparatus of claim 1, comprising a cryogenic heat exchanger with one or more tubings.
6) The apparatus of claim 5, where in the cryogenic heat exchanger comprises one or more tubings including redundant tubings.
7) The apparatus of claim 5, wherein the cryogenic heat exchanger comprises U-shaped tubings covering at least three walls of the payload bay.
8) The apparatus of claim 5, wherein the cryogenic heat exchanger comprises tubings covering at least four sides of the payload bay.
9) The apparatus of claim 5, wherein the cryogenic heat exchanger comprises a port coupled to one or more tubings to provide input and output connections thereto.
10) The apparatus of claim 5, comprising a door coupled to the payload bay, wherein the door comprises three or more materials having different thermal characteristics.
11) A method to provide ultra low temperature processing and/or storage, comprising:
a) providing insulation and structural support using a material disposed in a vacuum region between an external housing and an inner housing; and
b) cryogenically processing one or more compartments contained in a payload bay.
12) The method of claim 11, wherein the material comprises an insulation material with silica micro balloon technology.
13) The method of claim 11, comprising removing water vapor, partial pressure contaminates and atmospheric gases from the vacuum region.
14) The method of claim 11, comprising evacuating the vacuum region to approximately 0.2 millitorr.
15) The method of claim 11, wherein the cryogenic heat exchanger comprises one or more heat exchange tubings.
16) The method of claim 11, wherein the cryogenic heat exchanger comprises primary heat exchange tubings including redundant tubings.
17) The method of claim 16, wherein the redundant tubings comprise one of: tubings branched from the primary heat exchange tubings, tubings operating in parallel with the primary heat exchange tubings, U-shaped tubings covering at least three walls of the inner housing.
18) The method of claim 11, comprising providing a door adapted to seal a chamber in the payload bay, wherein the door comprises a plurality of materials each having different thermal characteristics.
19) The method of claim 11, comprising providing a changeable rack assembly in the chamber.
20) The method of claim 19, comprising transmitting energy from the payload bay into the heat exchanger through the changeable rack assembly.
21) The method of claim 11, comprising providing a negative pressure in the payload bay.
22) The method of claim 21, comprising providing pneumatic seals on the main door assembly and cryogenics vacuum pumping through the heat exchanger to remove thermal energy from the payload bay and into the heat exchanger.
23) The method of claim 1, wherein at least one of the external housing and the inner housing comprises a flat surface.
US13/731,013 2007-11-02 2012-12-30 Thermal insulation technique for ultra low temperature cryogenic processor Abandoned US20140013778A1 (en)

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US11/934,696 US7823394B2 (en) 2007-11-02 2007-11-02 Thermal insulation technique for ultra low temperature cryogenic processor
US12/984,206 US8541623B2 (en) 2011-01-04 2011-01-04 Oxidation method and reactor
US13/731,013 US20140013778A1 (en) 2007-11-02 2012-12-30 Thermal insulation technique for ultra low temperature cryogenic processor

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PT2471765E (en) 2015-10-14
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US20130343962A1 (en) 2013-12-26
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AU2011353661A1 (en) 2013-07-25
US8541623B2 (en) 2013-09-24
BR112013017263A2 (en) 2016-10-25
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MX346609B (en) 2017-03-27
CN103402622A (en) 2013-11-20
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CL2013001970A1 (en) 2014-06-13
US20120172629A1 (en) 2012-07-05
WO2012094078A1 (en) 2012-07-12
CA2823635C (en) 2019-09-10
EP2471765A1 (en) 2012-07-04
PL2471765T3 (en) 2015-11-30

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