Apparatus described herein include, but are not limited to: a structural region fabricated from a heat-sensitive material, the structural region including an outer wall and an inner wall with a gas-sealed gap between the outer wall and the inner wall; an activation region fabricated from a heat-resistant material, the activation region including one or more getters; a connector attached to the structural region and to the activation region, the connector including a flexible region and a region configured for sealing and detachment of the structural region from the activation region; and a vacuum pump operably attached to the connector.
Methods described herein include, but are not limited to: establishing vacuum within a gas-sealed apparatus including at least one activation region fabricated from a heat-resistant material, a structural region fabricated from a heat-sensitive material, and a connector between the regions; heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region, while maintaining the established vacuum within the gas-sealed apparatus; allowing the at least one activation region and the one or more getters to cool to a temperature compatible with structural stability of the heat-sensitive material; transferring the cooled one or more getters from the cooled at least one activation region to the structural region through the connector, while maintaining the established vacuum within the apparatus; and separating the connector between the regions while maintaining the vacuum within the structural region including the cooled one or more getters. Methods of establishing and maintaining vacuum within a storage device also include, but are not limited to: assembling substantially all structural components of a storage device, including an outer wall and an inner wall substantially defining a gas-sealed gap; attaching the storage device to a gas-sealed apparatus, the gas-sealed apparatus including a getter activation region containing one or more getters, a vacuum pump, and a connector operably connecting the storage device to the gas-sealed apparatus; activating the vacuum pump to establish gas pressure below atmospheric pressure within the gas-sealed gap of the storage device; heating the storage device to a predetermined temperature for a predetermined length of time; heating the getter activation region and the one or more getters to an activation temperature for an activation time suitable to activate one or more getters within the at least one getter activation region, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device; allowing the getter activation region and the one or more getters to cool to a predetermined temperature; flexing the connector to move the storage device and the getter activation region into a relative position wherein the getter activation region is above the storage device and the connector is substantially linear; allowing the getters to fall along the connector interior into the gas-sealed gap in the storage device, while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device; separating the connector at a location adjacent to the storage device while maintaining the established gas pressure below atmospheric pressure within the gas-sealed gap of the storage device. In addition to the foregoing, other method aspects are described in the claims, drawings, and text forming a part of the present disclosure.
In addition to the foregoing, other aspects are described in the claims, drawings, and text forming a part of the present disclosure. The foregoing summary is illustrative only and is not intended to be in any way limiting. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features will become apparent by reference to the drawings and the following detailed description.
In the following detailed description, reference is made to the accompanying drawings, which form a part hereof. In the drawings, similar symbols typically identify similar components, unless context dictates otherwise. The illustrative embodiments described in the detailed description, drawings, and claims are not meant to be limiting. Other embodiments may be utilized, and other changes may be made, without departing from the spirit or scope of the subject matter presented here.
The use of the same symbols in different drawings typically indicates similar or identical items.
Methods and apparatus described herein are useful to establish and maintain a stable and extremely low gas pressure within an internal, gas-sealed region of a container. Methods and apparatus as described herein have a variety of potential uses in the manufacture of containers that include internal, gas-sealed regions with durable gas pressure below atmospheric pressure, such as near-vacuum gas pressure, without active pumping of gas out of the internal gas-sealed regions. Methods and apparatus described herein may be utilized to establish and maintain a durable low gas pressure region internal to a container structure, and may be particularly useful in regard to containers fabricated from materials that lose their structural stability at temperatures below the activation temperatures required by many getter materials. For example, the methods and apparatus as described herein may be utilized to establish and maintain a stable gas pressure below atmospheric pressure, such as near-vacuum gas pressure, within an internal, gas-sealed cavity within a portion of a larger device fabricated all or in part from aluminum. For example, the methods and apparatus as described herein may be useful in the manufacture and durability of containers fabricated out of plastic-metal composites that include internal, gas-impermeable spaces with gas pressure less than that of the environment surrounding the container, such as substantially evacuated, gas-impermeable internal spaces.
Internal, gas-sealed regions with low gas pressure may be incorporated into the structure of containers as part of the insulation for the container. Internal, gas-sealed regions of low gas pressure incorporated into the structure of containers as partial insulation for the container may include other materials or features, such as insulation materials, electronics or structural features of the container. For example, internal, gas-sealed regions of low gas pressure incorporated into the structure of a container may include multilayer insulation material (MLI). For example, internal, gas-sealed regions of low gas pressure incorporated into the structure of a container may include wires or conduits connecting electronic components operably attached to different regions of the container. Internal, gas-sealed regions of low gas pressure may also isolate electronics incorporated into the device from external factors, such as chemically active materials, magnetically active materials, water, heat and cold. For example, internal, gas-sealed regions of low gas pressure incorporated into the structure of a container may include structural elements such as flanges, supports, struts and other features improving the structural stability of the container. Internal, gas-sealed regions of low pressure may have advantages of low weight and cost in a finished, manufactured device. Methods and apparatus described herein may be used to manufacture substantially thermally sealed storage devices, such as those suitable for stable maintenance of stored materials within a predetermined temperature range without reliance on external power sources to maintain the temperature range within the storage area. For example, containers and devices such as those manufactured with the methods and apparatus described herein are suitable for maintenance of stored materials within a predetermined temperature range in locations with minimal municipal power, or unreliable municipal power sources, such as remote locations or in emergency situations. For example, containers and devices such as those manufactured with the methods and apparatus described herein may be useful for the transport and storage of materials that are sensitive to external temperature changes that can occur during shipment and storage. For example, the storage systems described herein are useful for the shipment and storage of medicinal agents, including vaccines.
Many medicinal agents, including vaccines, currently in regular use are highly sensitive to temperature variations, and must be maintained in a particular temperature range to preserve stability, as well as the potency and efficacy of the medicinal agents. The temperature range to maintain stability in storage is inherent to the particular formulation and medicinal agent. For example, many medicinal agents, including vaccines, must be stored in a predetermined temperature range, such as between 2 degrees Centigrade and 8 degrees Centigrade, or between 0 degrees Centigrade and 10 degrees Centigrade, or between 10 degrees Centigrade and 15 degrees Centigrade, or between 15 degrees Centigrade and 25 degrees Centigrade, or between −15 degrees Centigrade and −5 degrees Centigrade, or between −50 degrees Centigrade and −15 degrees Centigrade, to preserve efficacy of the medicinal agent. Storage and transport of medicinal agents, including vaccines, within a temperature range, such as between 2 degrees Centigrade and 8 degrees Centigrade, or between 0 degrees Centigrade and 10 degrees Centigrade, or between 10 degrees Centigrade and 15 degrees Centigrade, or between 15 degrees Centigrade and 25 degrees Centigrade, or between −15 degrees Centigrade and −5 degrees Centigrade, or between −50 degrees Centigrade and −15 degrees Centigrade, is often referred to as the “cold chain.”
Health care providers and clinics who use medicinal agents, such as vaccines, must follow established protocols and procedures for maintenance of the cold chain, including during transport and in times of emergency and in power failures, to ensure medicinal agent activity such as vaccine potency. See: Rodgers et al., “Vaccine Cold Chain Part 1 Proper Handling and Storage of Vaccine,” AAOHN Journal 58(8) 337-344 (2010); Rodgers et al., “Vaccine Cold Chain Part 2: Training Personnel and Program Management,” AAOHN Journal 8(9): 391-402 (2010); Magennis et al., “Pharmaceutical Cold Chain” A Gap in the Last Mile,” Pharmaceutical & Medical Packaging News, 44-50 (September 2010); and Kendal et al., “Validation of Cold Chain Procedures Suitable for Distribution of Vaccines by Public Health Programs in the USA,” Vaccine 15 (12/13): 1459-1465 (1997) which are each incorporated by reference. For example, failure to follow established protocols and procedures for maintenance of the cold chain, even during periods of normal use in developed countries, leads to significant levels of vaccine wastage due to exposure to both excessively high and excessively low temperatures. In some cases, a brief period outside of normal storage temperatures is sufficient to disrupt activity. See: Thakker and Woods, “Storage of Vaccines in the Community: Weak Link in the Cold Chain?” British Medical Journal 304: 756-758 (1992); Matthias et al., “Freezing Temperatures in the Vaccine Cold Chain: A Systematic Literature Review,” Vaccine 25: 3980-3986 (2007); Edsam et al., “Exposure of Hepatitis B Vaccine to Freezing Temperatures During Transport to Rural Health Centers in Mongolia,” Preventative Medicine 39: 384-388 (2004); Techathawat et al., “Exposure to Heat and Freezing in the Vaccine Cold Chain in Thailand,” Vaccine 25: 1328-1333 (2007); and Setia et al., “Frequency and Causes of Vaccine Wastage,” Vaccine 20: 1148-1156 (2002), which are each incorporated by reference. Although some breaks in cold chain maintenance, such as frozen vaccine vials and vials containing precipitants due to improper temperature exposure, may be readily apparent, medicinal agents such as vaccines with reduced potency due to breaks in cold chain maintenance may not be readily detectable. See: Chen et al., “Characterization of the Freeze Sensitivity of a Hepatitis B Vaccine,” Human Vaccines 5(1): 26-32 (2009), which is incorporated by reference. Medicinal agent stocks with reduced potency or efficacy due to exposure to excessively high temperatures may not be immediately identifiable. The temperature sensitivity of any given medicinal agent varies widely depending on the specific agent, or example the specific vaccine formulation. In some circumstances, a few minutes outside of the appropriate temperature range can significantly impact the biological effectiveness of a particular container of a medicinal agent. See: Kristensen and Chen, “Stabilization of Vaccines: Lessons Learned,” Human Vaccines 6(3): 229-230 (2010), which is incorporated by reference. Issues related to the maintenance of cold chain are even more significant in less well developed regions of the world. See: Wirkas et al., “A Vaccine Cold Chain Freezing Study in PNG Highlights Technology Needs for Hot Climate Countries,” Vaccine 25: 691-697 (2007); and Nelson et al., “Hepatitis B Vaccine Freezing in the Indonesian Cold Chain: Evidence and Solutions,” Bulletin of the World Health Organization, 82(2): 99-105 (2004), which are each incorporated by reference. In addition, approaches to the cold chain that require less energy may be desirable for ongoing cost and climate considerations. See Halldórsson and Kovacs, “The Sustainable Agenda and Energy Efficiency: Logistics Solutions and Supply Chains in Times of Climate Change,” International Journal of Physical Distribution & Logistics Management 40 (1/2): 5-13 (2010), which is incorporated by reference. Thermal stabilization of medicinal agents, such as vaccines, for use beyond the cold chain includes economic, logistical, regulatory, procurement and policy issues (see Kristensen and Chen, “Stabilization of vaccines: lessons learned,” Human Vaccines, vol. 6, no. 3, March 2010, pages 229-231, which is incorporated by reference).
Containers and storage devices such as those fabricated using methods and apparatus described herein may be designed in a variety of sizes and shapes, depending on the embodiment. For example, containers and storage devices may be fabricated in various sizes, shapes and materials depending on the intended use of the container or storage device. A representative example of a storage container is shown in
With reference now to
The structural region 180 is fabricated from a heat-sensitive material. The structural region 180 may be fabricated entirely or in part from a heat-sensitive material. The structural region 180 may be fabricated from a combination of materials. Wherein the structural region includes components fabricated from different materials, the material with the lowest heat tolerance will govern the heat-sensitivity of the entire structural region 180. The structural region 180 includes an outer wall 150 and an inner wall 155, with a gas-sealed gap 145 between the outer wall 150 and the inner wall 155. The activation region 100 is fabricated from a heat-resistant material. The activation region 100 is entirely fabricated from a heat-resistant material utilizing methods that are also heat-resistant. For example, any epoxy, seals, coatings or similar components within the activation region 100 structure will be heat-resistant. Wherein the activation region includes components fabricated from different materials, the material with the lowest heat tolerance will govern the heat-resistance of the entire activation region 100. The activation region 100 includes one or more getters 110.
The connector 120 is attached to both the structural region 180 and the activation region 100. The connector 120 is operably connected to both the structural region 180 and the activation region 100 with gas-impermeable connections to form a gas-sealed interior. For example, the connector 120 may be attached to the structural region 180 and the activation region 100 using gas-impermeable seals on the respective ends of the connector 120. For example, the connector 120 may be welded on to the structural region 180 and the activation region 100 on the respective ends of the connector 120 to form a gas-impermeable welding joint. The connector 120 includes a flexible region 125. The connector includes a region 127 configured for sealing and detachment of the structural region 180 from the activation region 100. The vacuum pump 130 is operably attached to the connector 120. The vacuum pump 130 is operably attached to the connector 120 to allow the vacuum pump 130 to substantially evacuate the gas within the gas-sealed interior of the apparatus 185 during utilization of the methods described herein. In some embodiments, the vacuum pump 130 may be operably attached to the connector 120 through a tube, duct, conduit or other structure that creates a gas-impermeable seal between the vacuum pump 130 and the connector 120.
The apparatus 185 includes a gas-sealed interior region throughout the structural region 180, the activation region 100, and the connector 120 attached to the structural region 180 and to the activation region 100. Gas-impermeable seals are located in each of the junctions between regions 180, 100 of the apparatus 185 and the connector. The vacuum pump 130 is also operably attached to the connector 120 with a gas-impermeable seal. See: Ishimaru, “Bakable aluminum vacuum chamber and bellows with an aluminum flange and metal seal for ultrahigh vacuum,” Journal of Vacuum Science and Technology, vol. A15, no. 6, November/December 1978, pages 1853-1854; and Jhung et al., “Achievement of extremely high vacuum using a cryopump and conflate aluminum gaskets,” Vacuum, vol. 43, no. 4, 1992, pages 309-311; which are each incorporated by reference. The vacuum pump 130 may be attached to the connector 120 through a through a structure, such as conduit 170, that includes a gas-impermeable seal between the vacuum pump 130 and the connector 120. The vacuum pump 130 included in a specific embodiment should have sufficient pumping capacity to substantially evacuate the entirety of the gas-sealed interior region throughout the structural region 180, the activation region 100, and the connector 120 attached to the structural region 180 and to the activation region 100.
A valve 135 may be operably attached to the connector 120, for example in the region of the connector 120 between the attached vacuum pump 130 and conduit 170 and the attached structural region 180. A valve 135 operably attached to the connector 120 may be configured to inhibit the flow of gas through the connector 120. A valve 135 operably attached to the connector 120 may be configured to block the flow of gas through the connector 120. A valve 135 operably attached to the connector 120 is configured to restrict gas flow through the interior of the connector 120 at a location along the length of the connector 120. For example, as illustrated in
The structural region 180 fabricated from a heat-sensitive material includes a device configured for use independently from the remainder of the apparatus. For example, the structural region 180 may include a storage device (see, e.g.
The structural region 180 fabricated from a heat-sensitive material may be fabricated from a variety of heat-sensitive materials, depending on the embodiment. The structural region 180 may be fabricated to include a single heat-sensitive material. The structural region 180 fabricated from a heat-sensitive material may be fabricated from a plurality of materials, one or more of which may be heat-sensitive, depending on the embodiment. For example, the structural region 180 may be fabricated partially or entirely from aluminum. The structural region 180 may include a plurality of materials in a particular embodiment. The structural region 180 may be fabricated from composite materials. For example, the structural region 180 may be fabricated partially or entirely from metalized plastic, such as polypropylene, PET, nylon or polyethylene completely covered with a layer of metal, such as aluminum, on the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145. For example, the structural region 180 may be fabricated partially or entirely from plastic with a metal coating, or from plastic with a metal liner, on the interior surface of the gas-sealed gap 145 (e.g. as illustrated as surfaces 190 in
In order to maintain a low gas pressure within the gas-sealed gap 145, in some embodiments the structural region 180 is fabricated entirely or partially from low vapor emitting materials. For example, the structural region 180 may be fabricated from low vapor-emitting materials such as aluminum, stainless steel, or other metals. For example, the structural region 180 may be fabricated from low vapor-emitting materials such as glass or appropriate ceramics. In order to maintain a low gas pressure within the gas-sealed gap 145, in some embodiments the structural region 180 is fabricated with a layer of low vapor emitting materials on the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145. For example, the surfaces 190 may be covered with a layer of stainless steel, aluminum, or other low vapor emitting material. In some embodiments the surfaces 190 of the outer wall 150 and the inner wall 155 facing the gas-sealed gap 145 is cleaned and treated prior to assembly to reduce the sublimation of contaminants (e.g. water, oils, or plastics) from the surfaces 190 into the gas-sealed gap 145 (see
The materials used to fabricate the components of the apparatus 185, as well as any treatment of the components prior to assembly of the apparatus 185 (see, e.g.,
The term “heat-sensitive,” as used herein, refers to materials that lose their structural integrity at temperatures below the activation temperature(s) and under the activation condition(s) for the types of getter(s) 110 used in the apparatus 185. The term “heat-sensitive,” as used herein, is relative to the activation temperature(s) and the pressure conditions used for the specific getters 110 included in a given embodiment. For example, in some embodiments the getters 110 included in the apparatus 185 may include zirconium-vanadium-iron getters (see U.S. Pat. No. 4,312,669 “Non-evaporable Ternary Gettering Alloy and Method of Use for the Sorption of Water, Water Vapor and Other Gasses,” to Boffito et al., which is incorporated by reference). For example, in some embodiments the getters 110 included in the apparatus 185 may include St707™ getters with 70% zirconium, 24.6% vanadium and 5.4% iron (for example, available from Getter Technologies International Ltd., China). See also Hobson and Chapman, “Pumping of methane by St707 at low temperatures,” Journal of Vacuum and Science Technology,” vol. A4, no. 3, May/June 1986, pages 300-302, which is incorporated by reference. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature of approximately 700 degrees Centigrade for at least 20 seconds and then reducing the temperature to between approximately 400 degrees Centigrade and approximately 25 degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. A “heat-sensitive material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would be a heat-sensitive material that is predicted to lose its structural integrity in a temperature of approximately 700 degrees Centigrade lasting for at least 20 seconds. A “heat-sensitive material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would lose its structural integrity at a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. For example, in some embodiments the structural region 180 is fabricated from a heat-sensitive material that includes aluminum, or aluminum alloy that loses its structural integrity at temperatures above 250 degrees Centigrade. See: Ishimaru et al., “New all aluminum alloy vacuum system for the TRISTAN e+e− storage accelerator,” IEEE Transactions on Nuclear Science, Vol. NS-28, no. 3, 1981, pages 3320-3322, which is incorporated by reference.
The term “structural integrity,” as used herein, refers to a structure maintaining its fabricated form in a set of given conditions. Loss of structural integrity, correspondingly, refers to the failure of a structure to maintain its fabricated form in a set of conditions. “Heat-sensitive” materials, as used herein, refers to materials that lose their structural integrity at temperatures below the activation temperature(s) and under the activation condition(s) for the types of getter(s) 110 used in an embodiment of an apparatus 185. Conditions affecting loss of structural integrity may include temperature ranges, such as excessively hot or cold temperatures, and gas pressures, such as minimal gas pressure within an interior region. Conditions affecting loss of structural integrity may include conditions of intended use, such as weight-bearing, erosion, compressive strength, or tensile strength. Loss of structural integrity may be overt or gross, such as when a structure in whole or part melts, deforms, distorts, implodes, or combusts. Loss of structural integrity may include a change the outgassing properties of a material used in fabrication of a structure, for example a plastic material with low outgassing properties may exhibit increased outgassing properties in a set of given conditions, such as temperature or gas pressure. Loss of structural integrity may also be inconspicuous or undetectable to a cursory inspection, such as in the formation of a small hole, surface thinning, alteration of a crystalline or other non-overt structure of a fabricated material, or loss of cohesion at a weld or joint. For example, in some embodiments, aluminum and aluminum alloys are “heat-sensitive,” as used herein, and may lose their structural integrity in some conditions required to activate some types of getters employed in the specific embodiment. For example, although aluminum and aluminum alloys may not completely melt into a liquid form at temperatures above 250 degrees Centigrade, in some instances they will begin to soften and, as such, lose their structural integrity. Similarly, copper and copper alloys may be considered heat-sensitive materials in some embodiments. See Koyatsu et al., “Measurements of outgassing rate from copper and copper alloy chambers,” Vacuum, vol. 47, no. 6-8, 1996, pages 709-711, which is incorporated by reference. When combined with the force of gravity on the structural region 180 and any force due to a low gas pressure within the gas-sealed gap 145, aluminum and aluminum alloys at temperatures above 250 degrees Centigrade may lose their structural integrity and manufactured form and compress, shift, or bend. Similarly, plastic and plastic composites used in some embodiments may be heat sensitive materials.
As illustrated in
In some embodiments, the gas-sealed gap 145 includes additional material. In some embodiments, the gas-sealed gap 145 includes additional material designed to improve the durability and stability of the structural region 180. For example, the gas-sealed gap 145 may include structural features, such as one or more flanges, struts, braces, crossbars, or posts that may be configured to maintain the stability of the structural region 180. For example, the gas-sealed gap 145 may include internal support structure, such as reinforced regions of the inner wall 155 and the outer wall 150.
In some embodiments, the gas-sealed gap 145 includes additional insulating material that improves the thermal properties of the structural region 180. For example, the gas-sealed gap 145 may include multilayer insulation material (MU). See: Wiedmann et al., “Multi Layer Insulation Literature,” DLR, Institute of Structural Mechanics, 20 pages total; Wei et al., “Effects of structure and shape on thermal performance of perforated multi-layer insulation blankets,” Applied Thermal Engineering, vol. 29, 2009, pages 1264-1266; Halaczek and Rafalowicz, “Heat transport in self-pumping multilayer insulation,” Cryogenics, vol. 26, 1986, pages 373-376; Shu et al., “Heat flux from 277 to 77 K through a few layers of multilayer insulation,” Cryogenics vol. 26, 1986, pages 671-677; Jacob et al., “Investigations into the thermal performance of multilayer insulation (300-77 K) Part 1: calorimetric studies,” Cryogenics, vol. 32, no. 12, 1992, pages 1137-1146; Jacob et al., “Investigations into the thermal performance of multilayer insulation (300-77 K) Part 2: Thermal analysis,” Cryogenics, vol. 32, no. 12, 1992, pages 1147-1153; Halaczek and Rafalowicz, “Unguarded cryostat for thermal conductivity measurements of multilayer insulations,” Cryogenics, vol. 25, 1985, pages 529-530; Mikhalchenko et al., “Theoretical and experimental investigation of radiative-conductive heat transfer in multilayer insulation,” Cryogenics, vol. 25, 1985, pages 275-278; Bapat et al., “Experimental investigations of multilayer insulation,” Cryogenics, vol. 30, 1990, pages 711-719; U.S. Pat. No. 5,590,054 to McIntosh, titled “Variable-density method for multi-layer insulation;” Zhitomirskil et al., “A theoretical model of the heat transfer process in multilayer insulation,” Cryogenics, 1979, pages 265-268; Shu, “Systematic study to reduce the effects of cracks in multilayer insulation Part 1: theoretical model,” Cryogenics, vol. 27, 1987, pages 249-256; Shu, “Systematic study to reduce the effects of cracks in multilayer insulation Part 2: experimental results,” Cryogenics, vol. 27, 1987, pages 298-311; Glassford and Liu, “Outgassing rate of multilayer insulation,” Lockheed Palo Alto Research Laboratory, pages 83-106; Halaczak and Rafalowicz, “Flat-plate cryostat for measurements of multilayer insulation thermal conductivity,” Cryogenics, vol. 25, 1985, pages 593-595; Matsuda and Yoshikiyo, “Simple structure insulating material properties for multilayer insulation,” Cryogenics, 1980, pages 135-138; Keller et al., “Application of high temperature multilayer insulations,” Acta Astronautica, vol. 26, no. 6, 1992, pages 451-458; Scurlock and Saull, “Development of multilayer insulations with thermal conductivities below 01. μW cm−1 K−1,” Cryogenics, May 1976, pages 303-311; Bapat et al., “Performance prediction of multilayer insulation,” Cryogenics vol. 30, 1990, pages 700-710; and Kropschot, “Multiple layer insulation for cryogenic applications,” Cryogenics, 1961, pages 171-177; which are each incorporated by reference.
In some embodiments, there is at least one section of ultra efficient insulation material within the gas-sealed gap 145. The term “ultra efficient insulation material,” as used herein, may include one or more type of insulation material with extremely low heat conductance and extremely low heat radiation transfer between the surfaces of the insulation material. The ultra efficient insulation material may include, for example, one or more layers of thermally reflective film, high vacuum, aerogel, low thermal conductivity bead-like units, disordered layered crystals, low density solids, or low density foam. In some embodiments, the ultra efficient insulation material includes one or more low density solids such as aerogels, such as those described in, for example: Fricke and Emmerling, Aerogels—preparation, properties, applications, Structure and Bonding 77: 37-87 (1992); and Pekala, Organic aerogels from the polycondensation of resorcinol with formaldehyde, Journal of Materials Science 24: 3221-3227 (1989), which are each herein incorporated by reference. As used herein, “low density” may include materials with density from about 0.01 g/cm3 to about 0.10 g/cm3, and materials with density from about 0.005 g/cm3 to about 0.05 g/cm3. In some embodiments, the ultra efficient insulation material includes one or more layers of disordered layered crystals, such as those described in, for example: Chiritescu et al., Ultralow thermal conductivity in disordered, layered WSe2 crystals, Science 315: 351-353 (2007), which is herein incorporated by reference. In some embodiments, the ultra efficient insulation material includes at least two layers of thermal reflective film surrounded, for example, by at least one of: high vacuum, low thermal conductivity spacer units, low thermal conductivity bead like units, or low density foam. See, for example, Mikhalchenko et al., “Study of heat transfer in multilayer insulation based on composite spacer materials,” Cryogenics, 1983, pages 309-311, which is incorporated by reference herein. In some embodiments, the ultra efficient insulation material may include at least two layers of thermal reflective material and at least one spacer unit between the layers of thermal reflective material. For example, the ultra-efficient insulation material may include at least one multiple layer insulating composite such as described in U.S. Pat. No. 6,485,805 to Smith et al., titled “Multilayer insulation composite,” which is herein incorporated by reference. For example, the ultra-efficient insulation material may include at least one metallic sheet insulation system, such as that described in U.S. Pat. No. 5,915,283 to Reed et al., titled “Metallic sheet insulation system,” which is herein incorporated by reference. For example, the ultra-efficient insulation material may include at least one thermal insulation system, such as that described in U.S. Pat. No. 6,967,051 to Augustynowicz et al., titled “Thermal insulation systems,” which is herein incorporated by reference. For example, the ultra-efficient insulation material may include at least one rigid multilayer material for thermal insulation, such as that described in U.S. Pat. No. 7,001,656 to Maignan et al., titled “Rigid multilayer material for thermal insulation,” which is herein incorporated by reference. See also: Li et al., “Study on effect of liquid level on the heat leak into vertical cryogenic vessels,” Cryogenics, vol. 50, 2010, pages 367-372; Barth et al., “Test results for a high quality industrial superinsulation,” Cryogenics, vol. 28, 1988, pages 607-609; and Eyssa and Okasha, “Thermodynamic optimization of thermal radiation shields for a cryogenic apparatus,” Cryogenics, 1978, pages 305-307; which are each incorporated by reference. For example, the ultra-efficient insulation material may include multilayer insulation material, or “MLI.” For example, an ultra efficient insulation material may include multilayer insulation material such as that used in space program launch vehicles, including by NASA. See, e.g., Daryabeigi, Thermal analysis and design optimization of multilayer insulation for reentry aerodynamic heating, Journal of Spacecraft and Rockets 39: 509-514 (2002), which is herein incorporated by reference. For example, the ultra efficient insulation material may include space with a gaseous pressure lower than atmospheric pressure external to the gas-sealed gap 145. See, for example, Nemanic, “Vacuum insulating panel,” Vacuum, vol. 46, nos. 8-10, 1995, pages 839-842, which is incorporated by reference. In some embodiments, the ultra efficient insulation material may substantially cover the inner wall 155 surface facing the gas-sealed gap 145. In some embodiments, the ultra efficient insulation material may substantially cover the outer wall 150 surface facing the gas-sealed gap 145.
In some embodiments, there is at least one layer of multilayer insulation material (“MLI”) within the gas-sealed gap 145. The at least one layer of multilayer insulation material may substantially surround the surface of the inner wall 155. In some embodiments, there are a plurality of layers of multilayer insulation material within the gas-sealed gap 145, wherein the layers may not be homogeneous. For example, the plurality of layers of multilayer insulation material may include layers of differing thicknesses, or layers with and without associated spacing elements. In some embodiments there may be one or more additional layers within or in addition to the insulation material, such as, for example, an outer structural layer or an inner structural layer. An inner or an outer structural layer may be made of any material appropriate to the embodiment, for example an inner or an outer structural layer may include: plastic, metal, alloy, composite, or glass. See, for example, U.S. Pat. No. 4,726,974 to Nowobilski et al., titled “Vacuum insulation panel,” which is incorporated by reference. In some embodiments, there may be one or more layers of high vacuum between layers of thermal reflective film. In some embodiments, the gas-sealed gap 145 includes a substantially evacuated gaseous pressure relative to the atmospheric pressure external to the structural region 180. A substantially evacuated gaseous pressure relative to the atmospheric pressure external to the structural region 180 may include substantially evacuated gaseous pressure surrounding a plurality of layers of MLI, for example between and around the layers. A substantially evacuated gaseous pressure relative to the atmospheric pressure external to the structural region 180 may include substantially evacuated gaseous pressure in one or more sections of the gas-sealed gap 145. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 1×10−2 torr. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 5×10−4 torr. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 1×10−2 torr in the gas-sealed gap 145. For example, in some embodiments the gas-sealed gap 145 includes substantially evacuated space having a pressure less than or equal to 5×10−4 torr in the gas-sealed gap 145. In some embodiments, the gas-sealed gap 145 includes substantially evacuated space having a pressure less than 1×10−2 torr, for example, less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr. For example, in some embodiments the gas-sealed gap 145 includes a plurality of layers of multilayer insulation material and substantially evacuated space having a pressure less than or equal to 1×10−2 torr. For example, in some embodiments the gas-sealed gap 145 includes a plurality of layers of multilayer insulation material and substantially evacuated space having a pressure less than or equal to 5×10−4 torr.
As illustrated in
The apparatus 185 includes an activation region 100 fabricated from a heat-resistant material, the activation region 100 including one or more getters 110. Although a single activation region 100 is depicted in
As used herein, the term “heat-resistant material” refers to materials that maintain their structural integrity at temperatures and conditions above the activation temperature(s) and within the condition(s) for the types of getter(s) 110 used in the apparatus 185. The term “heat-resistant,” as used herein, is relative to the activation temperature(s) and gas pressure conditions used for the specific getters 110 included in a given embodiment. For example, in some embodiments the getters 110 included in the apparatus 185 may include zirconium-vanadium-iron getters (see U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein). For example, in some embodiments the getters 110 included in the apparatus 185 may include St707™ getters with 70% zirconium, 24.6% vanadium and 5.4% iron (for example, available from Getter Technologies International Ltd., China). See: Gunter et al., “Microstructure and bulk reactivity of the nonevaporable getter Zr57V36Fe7,” Journal of Vacuum Science Technology, Vol. A16, no. 6, November/December 1998, pages 3526-3535, which is incorporated by reference. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature of approximately 700 degrees Centigrade for at least 20 seconds and then reducing the temperature to between approximately 400 degrees Centigrade and approximately 25 degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, a zirconium-vanadium-iron getter material may be activated by heating to a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. A “heat-resistant material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would be a heat-resistant material that is predicted to maintain its structural integrity in a temperature of approximately 700 degrees Centigrade lasting for at least 20 seconds. A “heat-resistant material,” as used herein, for use with an embodiment incorporating getters fabricated from a zirconium-vanadium-iron getter material, would conserve its structural integrity at a temperature less than 450 degrees Centigrade, such as approximately 400 degrees Centigrade, or between approximately 250 and approximately 350 degrees Centigrade, for a time between 1 and 10 minutes while in an environment with a gas pressure of less than 10−2 torr. For example, in some embodiments the getters 110 included in the apparatus 185 may include getters fabricated from a titanium-zirconium-vanadium getter material. See: Matolin and Johanek, “Static SIMS study of TiZrV NEG activation,” Vacuum, vol. 67, 2002, pages 177-184, which is incorporated by reference. A “heat-resistant material,” as used herein, for use with an embodiment incorporating getters fabricated from a titanium-zirconium-vanadium getter material, would conserve its structural integrity at a temperature less of approximately 300 degrees Centigrade with a gas pressure within the interior of approximately 5×10−11 mbar (see Matolin and Johanek, ibid, which is incorporated by reference). For example, in some embodiments the structural region 180 is fabricated from a heat-resistant material that includes stainless steel, or stainless steel alloys. For example, in some embodiments the structural region 180 is fabricated from a heat-resistant material that includes titanium alloy.
Getters of a variety of types may be used in different embodiments. The getters may be fabricated from a variety of getter materials. For example, the getters may be fabricated from non-evaporatable getter material. The selection of getters may depend, for example, on the availability, cost, mass, chemical composition, toxicity and durability of the getter material employed in a given embodiment. The selection of getters may depend, for example, on the activation temperature and conditions for a particular getter material. Some types of getters are activatable at different temperatures and gas pressure conditions for different lengths of time (see, e.g. U.S. Pat. No. 4,312,669 “Non-evaporable Ternary Gettering Alloy and Method of Use for the Sorption of Water, Water Vapor and Other Gasses,” to Boffito et al., which is incorporated by reference), and for such getter materials the selection of the materials may depend on the range of potential temperatures, gas pressure conditions, and times, or one or more combinations of activation temperatures, gas pressure conditions and times for a specific getter material. Some getters may require gas pressure conditions less than atmospheric pressures, such as near-vacuum conditions, during activation at particular temperatures (see Matolin and Johanek, ibid, and U.S. Pat. No. 4,312,669, ibid., which are each incorporated by reference). The selection of getters may depend, for example, on the operational temperature of a given getter material, such as within ambient temperatures (i.e. substantially between 20 degrees Centigrade and 30 degrees Centigrade), within refrigeration temperatures (i.e. substantially between 2 degrees Centigrade and 10 degrees Centigrade) or within freezing temperatures (for example, substantially between 0 degrees Centigrade and −10 degrees Centigrade, or substantially between −15 degrees Centigrade and −25 degrees Centigrade). Some embodiments may include a single type of getters, for example getters fabricated from substantially the same active getter material. Some embodiments may include a plurality of types of getters fabricated from substantially distinct getter materials. More information regarding types of getters and getter materials suitable for various embodiments of the invention may be found in: Tripathi et al., “Hydrogen intake capacity of ZrVFe alloy bulk getters,” Vacuum, vol. 48, no. 12, 1997, pages 1023-1025; Benvenuti et al., “Nonevaporable getter films for ultrahigh vacuum applications,” Journal of Vacuum and Science Technology, vol. A16, no. 1, January/February 1998, pages 148-154; Benvenuti et al., “Decreasing surface outgassing by thin film getter coatings,” Vacuum, vol. 50, nos. 1-2, 1998, pages 57-63; Boffito et al., “A nonevaporable low temperature activatable getter material,” Journal of Vacuum and Science Technology, vol. 18, no. 3, May/June 1981, pages 1117-1120; della Porta, “Gas problem and gettering in sealed-off vacuum devices,” Vacuum, vol. 47, nos 6-8, 1996, pages 771-777; Benvenuti and Chiggiato, “Obtention of pressures in the 10-14 torr range by means of a Zr—V—Fe non evaporable getter,” Vacuum, vol. 44, nos. 5-7, 1993, pages 511-513; Londer et al., “New high capacity getter for vacuum insulated mobile LH2 storage tank systems,” Vacuum, vol. 82, 2008, pages 431-434; Li et al., “Design and pumping characteristics of a compact titanium-vanadium non-evaporable getter pump,” Journal of Vacuum and Science Technology, vol. A16, no. 3, May/June 1998, pages 1139-1144; Chiggiato, “Production of extreme high vacuum with non evaporable getters,” Physica Scripta, vol. T71, 1997, pages 9-13; Benvenuit and Chiaggiato, “Pumping characteristics of the St707 nonevaporable getter (Zr 70 V 24.6-Fe 5.4 wt %),” Journal of Vacuum and Science Technology, vol. A14, no. 6, November/December 1996, pages 3278-3282; Day, “The use of active carbons as cryosorbent,” Colloids and Surfaces A: Physicochem. Eng. Aspects 187-188, 2001, pages 187-206; U.S. Pat. No. 4,312,669 “Non-evaporable Ternary Gettering Alloy and Method of Use for the Sorption of Water, Water Vapor and Other Gasses,” to Boffito et al.; Hobson and Chapman, “Pumping of methane by St707 at low temperatures,” Journal of Vacuum and Science Technology, vol. A4, no. 3, May/June 1986, pages 300-302; and Matolin and Johanek, “Static SIMS study of TiZrV NEG activation,” Vacuum, vol. 67, 2002, pages 177-184; which are each incorporated by reference.
As illustrated in
As noted herein, the apparatus 185 is configured to establish and maintain a reduced gas pressure environment within the gas-sealed gap 145 of the structural region 180. Accordingly, the one or more getters 110 may include non-evaporatable getter material. The one or more getters 110 may include zirconium, vanadium and iron. For example, the one or more getters 110 may include 70% zirconium, 24.6% vanadium and 5.4% iron. For example, the one or more getters 110 may include St707 getters (available, for example, from SAES Getters Group, with corporate headquarters in Lainate, Italy; see attached online brochure downloaded on Sep. 21, 2011, which is incorporated by reference herein). Similar getter materials are also available from other sources, such as Getter Technologies International Ltd., China.
As illustrated in
The connector may include a valve 135 configured to inhibit the flow of gas within the connector 120. Some embodiments may include more than one valve. As illustrated in
As illustrated in
As illustrated in
The apparatus 185 includes a region 127 of the connector 120 configured for sealing and detachment of the structural region 180 from the activation region 100. In some embodiments, the apparatus 185 includes a region 127 of the connector 120 configured for sealing and detachment of the connector 120 adjacent to the structural region 180 along the length of the connector 120. As illustrated in
The apparatus 185, as illustrated in
Correspondingly, the activation region 100 should be operably attached to the connector 120 in a manner to minimally impede the movement of the getters 110 out of the activation region 100 and into the internal region within the connector 120. The attachment should provide a sufficient seal to allow for the establishment and maintenance of a reduced gas pressure (e.g. less than or equal to 1×10−2 torr) within the interior of the apparatus 185 by the vacuum pump 130. For example, in embodiments where the apparatus is fabricated from metal, the activation region 100 may be attached to the connector 120 by weld junctions. These weld junctions should be sufficiently smooth and minimally facing on the interior of the apparatus 185 to provide minimal impedance of the getters 110 through the connector 120. Similarly, the structural region 180 should be operably attached to the connector 120 in a manner to minimally impede the movement of the getters 110 out of the interior of the connector 120 and into the gas-sealed gap 145 within the structural region 180.
The interior diameter of the connector 120, including within its own regions 125 and 127, as well as the interior diameter of any valve(s) (e.g. 135) opening(s) should be suitable for the passage of the getters 110 through the apparatus 185 between the activation region 100 and the gas-sealed gap 145 in the structural region 180. The size and shape of any particular getters 110 used should be less than the interior diameter of the connector 120 and any valve(s) (e.g. 135) utilized within the apparatus 185. The interior of the connector 120 and any valve(s) (e.g. 135) incorporated into the apparatus 185 should include minimal surfaces which may impede the movement of the getters 110 through the apparatus 185. For example, the interior of the connector 120 and any valve(s) (e.g. 135) should be substantially smooth, without sharp, jutting, or rough edges that may impede the getters 110. For example, the interior of the connector 120 and any valve(s) (e.g. 135) should be substantially free of internal elements, such as struts or braces, which may inhibit getters 110 travelling through the interior. Generally, the interior of the apparatus 185 should be designed and fabricated to allow for the direct movement of the getters 110 from the interior of the activation region 100 through the connector 120 and into the gas-sealed gap 145 in the structural region 180 when the activation region 100, connector 120 and the structural region 180 are appropriately oriented (i.e. as depicted in
The container depicted in
A storage container such as depicted in
Block 530 illustrates washing the components with detergents and water. A detergent washing step may reduce the presence of fine contaminants such as hydrocarbon oils and solvents, which may contribute to undesirable outgassing within the finished apparatus. See: R. Elsey, “Outgassing of vacuum materials-II,” Vacuum, vol. 25, 1975, pp. 347-361, which is incorporated by reference. As an example, hand dishwashing detergent (i.e. Dawn Advanced Power Dish Soap, manufactured by the Procter & Gamble Company) may be used to hand wash the components in warm tap water and a standard soft sponge. As an additional example, the detergent Alconox® may be used to clean the components in tap water (available from Alconox Inc., White Plains N.Y.). Optional block 540 depicts rinsing the washed components with deionized water (DI water). Optional block 550 illustrates blowing the components dry with dehumidified nitrogen gas, or a comparable inert gas. This step may reduce non-visible water molecules adhering to the surface of the components. See, for example: A. Berman, “Water vapor in vacuum systems,” Vacuum, vol. 47, no. 4, 1996, pages 327-332; J.-R. Chen et al., “Outgassing behavior of A6063-EX aluminum alloy and SUS 304 stainless steel,” Journal of Vacuum Science and Technology, vol. A5, no. 6, November/December 1987, pages 3422-3424; Y. C. Liu et al., “Thermal outgassing study on aluminum surfaces,” Vacuum, vol. 44, nos. 5-7, 1993, pages 435-437; Chen and Liu, “A comparison of outgassing rate of 304 stainless steel and A6063-EX aluminum alloy vacuum chamber after filling with water,” Journal of Vacuum Science and Technology, vol. A5, no. 2, March/April 1987, pages 262-264; Ishimaru et al., “Fast pump-down aluminum ultrahigh vacuum system,” Journal of Vacuum Science and Technology, vol. A10, no. 3, May/June 1992, pages 547-552; Miki et al., “Characteristics of extremely fast pump-down process in an aluminum ultrahigh vacuum system,” Journal of Vacuum Science and Technology, vol. A12, no. 4, July/August 1994, pages 1760-1766; and Chen et al., “Outgassing behavior on aluminum surfaces: water in vacuum systems,” Journal of Vacuum Science and Technology, vol. A12, no. 4, July/August 1994, pages 1750-1754, which are each incorporated by reference. In some embodiments, treatment with different types of gas may be included. See: Tatenuma et al., “Quick acquisition of clean ultrahigh vacuum by chemical process technology,” Journal of Vacuum Science and Technology, vol. All, no. 4, July/August 1993, pages 1719-1724; Tatenuma et al., “Acquisition of clean ultrahigh vacuum using chemical treatment,” Journal of Vacuum Science and Technology, vol. A16, no. 4, July/August 1998, pages 2693-2697; and L. C. Beavis, “Interaction of hydrogen with the surface of type 304 stainless steel,” Journal of Vacuum Science and Technology, vol. 10, no. 2, March/April 1973, pages 386-390; which are incorporated by reference. Block 560 depicts baking the components under vacuum conditions. See, for example: H. Ishimaru, “Fast pump-down aluminum ultrahigh vacuum system,” Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 10, May 1992, p. 547, which is incorporated by reference.
Baking components under vacuum conditions has been demonstrated to be useful for reducing outgassing from some materials, for example, for aluminum and stainless steel components. See: J. Young, “Outgassing Characteristics of Stainless Steel and Aluminum with Different Surface Treatments,” Journal of Vacuum Science and Technology, 1969; Odaka and Ueda, “Dependence of outgassing rate on surface oxide layer thickness in type 304 stainless steel before and after surface oxidation in air,” Vacuum, no. 47, nos. 6-8, 1996, pages 689-692; Odaka et al., “Effect of baking temperature and air exposure on the outgassing rate of type 316L stainless steel,” Journal of Vacuum Science and Technology, vol. A5, no. 5, September/October 1987, pages 2902-2906; Zajec and Nemanic, “Hydrogen bulk states in stainless-steel related to hydrogen release kinetics and associated redistribution phenomena,” Vacuum, vol. 61, 2001, pages 447-452; Bernardini et al., “Air bake-out to reduce hydrogen outgassing from stainless steel,” Journal of Vacuum Science and Technology, vol. A16, no. 1, January/February 1998, pages 188-193; Nemanic et al., “Anomalies in kinetics of hydrogen evolution from austenitic stainless steel from 300 to 1000° C.,” Journal of Vacuum Science and Technology, vol. A19, no. 1, January/February 2001, pages 215-222; Nemanic and Bogataj, “Outgassing of thin wall stainless steel chamber,” Vacuum, vol. 50, no. 3-4, 1998, pages 431-437; Cho et al., “Creation of extreme high vacuum with a turbomolecular pumping system: a baking approach,” Journal of Vacuum Science and Technology, vol. A13, no. 4, July/August 1995, pages 2228-2232; and Y. Ishikawa and K. Odaka, “Reduction of outgassing from stainless surfaces by surface oxidation,” Vacuum, vol. 41, 1990, pp. 1995-1997; which are incorporated by reference. For example, stainless steel components may be baked for 30 hours at 250 degrees Centigrade in a chamber with a gas pressure of approximately 1×10−2 torr. As an additional example, aluminum components or composite components may be baked at 150 degrees Centigrade for 60-70 hours in a chamber with a gas pressure of approximately 1×10−2 torr. See also: Chen et al., “An aluminum vacuum chamber for the bending magnet of the SRRC synchrotron light source,” Vacuum, vol. 41, nos. 7-9, 1990, pages 2079-2081; Burns et al., “Outgassing test for non-metallic materials associated with sensitive optical surfaces in a space environment,” Materials and Processes Laboaratory, George C. Marshall Space Flight Center, 1987; and Chen et al., “Thermal outgassing from aluminum alloy vacuum chambers,” Journal of Vacuum Science and Technology, vol. A3, no. 6, November/December 1985, pages 2188-2191, which are each incorporated by reference. In addition or alternately, baking components in the presence of inert gas has been demonstrated to be useful for reducing outgassing from some materials. In some embodiments, as an alternate to near-vacuum gas pressure conditions, the components are baked in the presence of inert gas, such as nitrogen.
After the components are cleaned and prepared, the components of the apparatus are assembled. A helium leak check may be performed to ensure that seals and/or junctions are sufficient to maintain reduced gas pressure conditions within the interior of the apparatus. In addition, the apparatus may be purged with dehydrated nitrogen gas during the check of the final assembly. See: K. Yamazaki, et al., “High-speed pumping to UHV,” Vacuum, vol. 84, December 2009, pp. 756-759; and Chun et al., “outgassing rate characteristic of a stainless-steel extreme high vacuum system,” Journal of Vacuum Science and Technology, vol. A14, no. 4, July/August 1996, pages 2636-2640; which are incorporated by reference.
In some embodiments, heating the apparatus components while establishing the vacuum may reduce the time required to establish vacuum, for example by increasing the rate of evaporation of traces of water on the surfaces of the interior of the apparatus. In order to heat the apparatus components while establishing the vacuum, the apparatus may be placed within an oven of suitable size and operating conditions. In addition or alternately, in order to heat the apparatus components while establishing the vacuum, the exterior surfaces of the apparatus may be wrapped with heat tape, and the base of the apparatus may be placed on a hot plate. Suitable heat tape for some embodiments includes, for example, insulated heat tapes and may include fiberglass heavy insulated heat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, Stafford Tex.). The gas-sealed apparatus may be heated, for example, in temperature increments to ensure even heating, to allow time to monitor the apparatus, to allow for maintenance of the low gas pressure within the interior, and to ensure that the apparatus does not over-heat. The apparatus may be heated, as an example, to approximately 130-150 degrees Centigrade in approximately 50 degree increments during establishment of vacuum within the gas-sealed apparatus. The apparatus may be heated, as an example, to approximately 180-220 degrees Centigrade in approximately 20 degree increments during establishment of vacuum within the gas-sealed apparatus. Depending on the embodiment, establishing the vacuum may take several days, even with heating of the apparatus components assisting in a reduction of the time required. For example, establishing the vacuum may take a time on the order of 5-7 days of continual action by the vacuum pump and heating of the apparatus components. Even after suitable cleaning and other preparation, outgassing of volatile materials from the internal surfaces of the gas-sealed apparatus is expected, and will increase the time required to reach a suitably low gas pressure for a given embodiment. For example, heating the gas-sealed apparatus will increase outgassing of material from the internal surfaces of the gas-sealed apparatus. Suitable gas pressure within the interior of the apparatus is established when a gas pressure gauge operably attached to the apparatus displays a reading in the range appropriate for the embodiment (e.g. a gas pressure less than 1×10−2 torr, less than 5×10−3 torr, less than 5×10−4 torr, less than 5×10−5 torr, less than 5×10−6 torr or less than 5×10−7 torr).
The method flowchart depicted in
Heating the at least one activation region to an activation temperature for an activation time suitable to activate one or more getters within the at least one activation region while maintaining the established vacuum within the apparatus may include heating the activation region independently from the remainder of the apparatus while the vacuum pump attached to the apparatus is operating. For example, the activation region may be heated with a heat source external to the apparatus. In some embodiments, in order to heat the activation region, the activation region exclusively to the remainder of the apparatus may be placed within an oven of suitable size, shape and properties. In some embodiments, in order to heat the activation region, the exterior surfaces of the activation region may be wrapped with heat tape. Suitable heat tape for some embodiments includes, for example, insulated heat tapes and may include fiberglass heavy insulated heat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, Stafford Tex.). Heating the activation region may include heating with a heat source in direct thermal contact with the activation region and not in direct thermal contact with the structural region and the connector of the gas-sealed apparatus. For example, if heat tape is used, a specific section of heat tape may be wrapped around the outer surface of the activation region and set to a temperature higher than any temperature setting for the remainder of the apparatus.
The method flowchart depicted in
As shown in
The flowchart depicted in
Block 1620 depicts attaching the storage device to an apparatus, the apparatus including a getter activation region containing one or more getters, a vacuum pump, and a connector operably connecting the storage device to the apparatus. For example, the assembled device may be attached to an apparatus with a substantially gas-impermeable junction to form an apparatus such as illustrated in
As shown in
One skilled in the art will recognize that the herein described components (e.g., operations), devices, objects, and the discussion accompanying them are used as examples for the sake of conceptual clarity and that various configuration modifications are contemplated. Consequently, as used herein, the specific exemplars set forth and the accompanying discussion are intended to be representative of their more general classes. In general, use of any specific exemplar is intended to be representative of its class, and the non-inclusion of specific components (e.g., operations), devices, and objects should not be taken limiting.
The herein described subject matter sometimes illustrates different components contained within, or connected with, different other components. It is to be understood that such depicted architectures are merely exemplary, and that in fact many other architectures may be implemented which achieve the same functionality. In a conceptual sense, any arrangement of components to achieve the same functionality is effectively “associated” such that the desired functionality is achieved. Hence, any two components herein combined to achieve a particular functionality can be seen as “associated with” each other such that the desired functionality is achieved, irrespective of architectures or intermedial components. Likewise, any two components so associated can also be viewed as being “operably connected”, or “operably coupled,” to each other to achieve the desired functionality, and any two components capable of being so associated can also be viewed as being “operably couplable,” to each other to achieve the desired functionality. Specific examples of operably couplable include but are not limited to physically mateable and/or physically interacting components, and/or wirelessly interactable, and/or wirelessly interacting components, and/or logically interacting, and/or logically interactable components.
While particular aspects of the present subject matter described herein have been shown and described, it will be apparent to those skilled in the art that, based upon the teachings herein, changes and modifications may be made without departing from the subject matter described herein and its broader aspects and, therefore, the appended claims are to encompass within their scope all such changes and modifications as are within the true spirit and scope of the subject matter described herein. It will be understood by those within the art that, in general, terms used herein, and especially in the appended claims (e.g., bodies of the appended claims) are generally intended as “open” terms (e.g., the term “including” should be interpreted as “including but not limited to,” the term “having” should be interpreted as “having at least,” the term “includes” should be interpreted as “includes but is not limited to,” etc.). It will be further understood by those within the art that if a specific number of an introduced claim recitation is intended, such an intent will be explicitly recited in the claim, and in the absence of such recitation no such intent is present. For example, as an aid to understanding, the following appended claims may contain usage of the introductory phrases “at least one” and “one or more” to introduce claim recitations. However, the use of such phrases should not be construed to imply that the introduction of a claim recitation by the indefinite articles “a” or “an” limits any particular claim containing such introduced claim recitation to claims containing only one such recitation, even when the same claim includes the introductory phrases “one or more” or “at least one” and indefinite articles such as “a” or “an” (e.g., “a” and/or “an” should typically be interpreted to mean “at least one” or “one or more”); the same holds true for the use of definite articles used to introduce claim recitations. In addition, even if a specific number of an introduced claim recitation is explicitly recited, those skilled in the art will recognize that such recitation should typically be interpreted to mean at least the recited number (e.g., the bare recitation of “two recitations,” without other modifiers, typically means at least two recitations, or two or more recitations). Furthermore, in those instances where a convention analogous to “at least one of A, B, and C, etc.” is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., “a system having at least one of A, B, and C” would include but not be limited to systems that have A alone, B alone, C alone, A and B together, A and C together, B and C together, and/or A, B, and C together, etc.). In those instances where a convention analogous to “at least one of A, B, or C, etc.” is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., “a system having at least one of A, B, or C” would include but not be limited to systems that have A alone, B alone, C alone, A and B together, A and C together, B and C together, and/or A, B, and C together, etc.). It will be further understood by those within the art that typically a disjunctive word and/or phrase presenting two or more alternative terms, whether in the description, claims, or drawings, should be understood to contemplate the possibilities of including one of the terms, either of the terms, or both terms unless context dictates otherwise. For example, the phrase “A or B” will be typically understood to include the possibilities of “A” or “B” or “A and B.”
With respect to the appended claims, those skilled in the art will appreciate that recited operations therein may generally be performed in any order. Also, although various operational flows are presented in a sequence(s), it should be understood that the various operations may be performed in other orders than those which are illustrated, or may be performed concurrently. Examples of such alternate orderings may include overlapping, interleaved, interrupted, reordered, incremental, preparatory, supplemental, simultaneous, reverse, or other variant orderings, unless context dictates otherwise. Furthermore, terms like “responsive to,” “related to,” or other past-tense adjectives are generally not intended to exclude such variants, unless context dictates otherwise.
With respect to the use of substantially any plural and/or singular terms herein, those having skill in the art can translate from the plural to the singular and/or from the singular to the plural as is appropriate to the context and/or application. The various singular/plural permutations are not expressly set forth herein for sake of clarity.
All of the above U.S. patents, U.S. patent application publications, U.S. patent applications, foreign patents, foreign patent applications and non-patent publications referred to in this specification and/or listed in any Application Data Sheet, are incorporated herein by reference, to the extent not inconsistent herewith.
While various aspects and embodiments have been disclosed herein, other aspects and embodiments will be apparent to those skilled in the art. The various aspects and embodiments disclosed herein are for purposes of illustration and are not intended to be limiting, with the true scope and spirit being indicated by the following claims.
The present application is related to and claims the benefit of the earliest available effective filing date(s) from the following listed application(s) (the “Related applications”) (e.g., claims earliest available priority dates for other than provisional patent applications or claims benefits under 35 USC §119(e) for provisional patent applications, for any and all parent, grandparent, great-grandparent, etc. applications of the Related application(s)). All subject matter of the Related applications and of any and all parent, grandparent, great-grandparent, etc. applications of the Related applications, including any priority claims, is incorporated herein by reference to the extent such subject matter is not inconsistent herewith. For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/001,757, entitled TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Dec. 11, 2007, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/006,088, entitled TEMPERATURE-STABILIZED STORAGE CONTAINERS WITH DIRECTED ACCESS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Dec. 27, 2007, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/006,089, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Dec. 27, 2007, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/008,695, entitled TEMPERATURE-STABILIZED STORAGE CONTAINERS FOR MEDICINALS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Jan. 10, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/012,490, entitled METHODS OF MANUFACTURING TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Jan. 31, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/077,322, entitled TEMPERATURE-STABILIZED MEDICINAL STORAGE SYSTEMS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William Gates; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Mar. 17, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/152,465, entitled STORAGE CONTAINER INCLUDING MULTI-LAYER INSULATION COMPOSITE MATERIAL HAVING BANDGAP MATERIAL AND RELATED METHODS, naming Jeffrey A. Bowers; Roderick A. Hyde; Muriel Y. Ishikawa; Edward K. Y. Jung; Jordin T. Kare; Eric C. Leuthardt; Nathan P. Myhrvold; Thomas J. Nugent Jr.; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood Jr. as inventors, filed May 13, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/152,467, entitled MULTI-LAYER INSULATION COMPOSITE MATERIAL INCLUDING BANDGAP MATERIAL, STORAGE CONTAINER USING SAME, AND RELATED METHODS, naming Jeffrey A. Bowers; Roderick A. Hyde; Muriel Y. Ishikawa; Edward K. Y. Jung; Jordin T. Kare; Eric C. Leuthardt; Nathan P. Myhrvold; Thomas J. Nugent Jr.; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood Jr. as inventors, filed May 13, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/220,439, entitled MULTI-LAYER INSULATION COMPOSITE MATERIAL HAVING AT LEAST ONE THERMALLY-REFLECTIVE LAYER WITH THROUGH OPENINGS, STORAGE CONTAINER USING SAME, AND RELATED METHODS, naming Roderick A. Hyde; Muriel Y. Ishikawa; Jordin T. Kare; and Lowell L. Wood, Jr. as inventors, filed Jul. 23, 2008, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/658,579, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William Gates; Zihong Guo; Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Feb. 8, 2010, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/927,981, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS WITH FLEXIBLE CONNECTORS, naming Fong-Li Chou; Geoffrey F. Deane; William Gates; Zihong Guo; Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Nov. 29, 2010, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 12/927,982, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS INCLUDING STORAGE STRUCTURES CONFIGURED FOR INTERCHANGEABLE STORAGE OF MODULAR UNITS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William Gates; Jenny Ezu Hu; Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Nov. 29, 2010, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 13/135,126, entitled TEMPERATURE-STABILIZED STORAGE SYSTEMS CONFIGURED FOR STORAGE AND STABILIZATION OF MODULAR UNITS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William Gates; Jenny Ezu Hu; Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Mark K. Kuiper; Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene; Mike Vilhauer; Charles Whitmer; Lowell L. Wood, Jr.; and Ozgur Emek Yildirim as inventors, filed Jun. 23, 2011, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date.For purposes of the USPTO extra-statutory requirements, the present application constitutes a continuation-in-part of U.S. patent application Ser. No. 13/199,439, entitled METHODS OF MANUFACTURING TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed Aug. 29, 2011, which is currently co-pending, or is an application of which a currently co-pending application is entitled to the benefit of the filing date. The United States Patent Office (USPTO) has published a notice to the effect that the USPTO's computer programs require that patent applicants reference both a serial number and indicate whether an application is a continuation, continuation-in-part, or divisional of a parent application. Stephen G. Kunin, Benefit of Prior-Filed Application, USPTO Official Gazette Mar. 18, 2003. The present Applicant Entity (hereinafter “Applicant”) has provided above a specific reference to the application(s) from which priority is being claimed as recited by statute. Applicant understands that the statute is unambiguous in its specific reference language and does not require either a serial number or any characterization, such as “continuation” or “continuation-in-part,” for claiming priority to U.S. patent applications. Notwithstanding the foregoing, Applicant understands that the USPTO's computer programs have certain data entry requirements, and hence Applicant has provided designation(s) of a relationship between the present application and its parent application(s) as set forth above, but expressly points out that such designation(s) are not to be construed in any way as any type of commentary and/or admission as to whether or not the present application contains any new matter in addition to the matter of its parent application(s).
Number | Date | Country | |
---|---|---|---|
Parent | 12001757 | Dec 2007 | US |
Child | 13200555 | US | |
Parent | 12006088 | Dec 2007 | US |
Child | 12001757 | US | |
Parent | 12006089 | Dec 2007 | US |
Child | 12006088 | US | |
Parent | 12008695 | Jan 2008 | US |
Child | 12006089 | US | |
Parent | 12012490 | Jan 2008 | US |
Child | 12008695 | US | |
Parent | 12077322 | Mar 2008 | US |
Child | 12012490 | US | |
Parent | 12152465 | May 2008 | US |
Child | 12077322 | US | |
Parent | 12152467 | May 2008 | US |
Child | 12152465 | US | |
Parent | 12220439 | Jul 2008 | US |
Child | 12152467 | US | |
Parent | 12658579 | Feb 2010 | US |
Child | 12220439 | US | |
Parent | 12927981 | Nov 2010 | US |
Child | 12658579 | US | |
Parent | 12927982 | Nov 2010 | US |
Child | 12927981 | US | |
Parent | 13135126 | Jun 2011 | US |
Child | 12927982 | US | |
Parent | 13199439 | Aug 2011 | US |
Child | 13135126 | US |