High emissivity freeze dryer plates

Abstract

The freeze dryer includes a shelf and a container, at least one of which includes a material having an emissivity of about 0.6 or more and about 1.0 or less. The shelf plate includes a plate body and a material layer disposed on one or more surfaces of the plate body or constituting one or more surfaces of the plate body, the material layer having an emissivity of about 0.6 or more and about 1.0 or less.

Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims priority to U.S. Patent Application No. 18 / 526,125, filed December 1, 2023, which claims the benefit of U.S. Provisional Patent Application No. 63 / 431,134, filed December 8, 2022. The entire disclosure of the above application is incorporated herein by reference.

[0002] Government funding This invention was made with United States Government support under Contract No. H92222-16-C-0081 awarded by the United States Department of Defense. The United States Government has certain rights in this invention.

[0003] The present disclosure relates to freeze dryers, and more particularly to plates, components, and elements used in and for constructing freeze dryers, one or more of which have high emissivity. [Background technology]

[0004] This section provides background information related to the present disclosure that is not necessarily prior art.

[0005] Lyophilization (also called freeze-drying) involves processes used to preserve materials (including, for example, biological materials and / or foods and / or pharmaceuticals) to increase their shelf life and improve their transportation and safe handling. Lyophilization is generally performed by freezing a material (which is usually liquid at ambient temperature and pressure) to form a solid material and placing it in a low-pressure, low-temperature environment sufficient to lower the solid material below its triple point. For example, for water, the triple point is the temperature (approximately 0.01°C) and pressure (approximately 0.00603 atm) at which all three phases of water (i.e., vapor, liquid, and ice) can exist in equilibrium. Lyophilization is performed below the triple point to allow the ice to change to vapor without entering a liquid phase. This change from ice to vapor is known as sublimation.

[0006] Freeze-drying of a solution is often performed using a freeze-dryer equipped with a shelf system (e.g., a hydraulic shelf system) configured to receive a container containing the solution. Freeze-drying of the solution in the container can be accelerated if the solution is frozen into a relatively thin solid layer (e.g., ice) having an average thickness of, for example, about 0.2 centimeters (cm) or more and about 2.5 centimeters (cm) or less. For example, using a thin ice layer for freeze-drying can reduce the distance that the sublimation surface (i.e., the boundary between the dry region of the layer (sometimes called cake) and the still-frozen region of the layer (sometimes called ice)) must travel to complete drying, and can also reduce the vapor flow resistance of the dry cake layer that remains after the sublimation surface has passed. However, during freeze-drying, not all regions of the thin ice layer dry at the same rate. For example, when the sublimation surface (defined by the length and width of the thin solid layer) is observed during the freeze-drying process, some regions may be completely dry in the depth (i.e., thickness) direction, while other regions may still contain solid matter (e.g., ice) near the plates (or shelves) of the freeze-dryer. This uneven drying is due, in part, to the non-uniformity of the thin, solid ice layer: for example, some regions of the thin ice layer may contain more amorphous structure and / or larger ice crystals than other regions of the thin ice layer. Summary of the Invention [Problem to be solved by the invention]

[0007] Uneven drying of various regions of the cake can result in uneven cake shrinkage. This uneven cake shrinkage often leads to buckling of the intermediate cake (the structure containing the portion that has not yet dried) against the freeze dryer plates. Buckling of the intermediate cake is problematic because the areas of the intermediate cake that are no longer in contact with the freeze dryer plates cannot efficiently receive heat conducted from the freeze dryer plates, thus slowing the drying of these areas and lengthening the overall drying cycle. Similar concerns about conductive heating can also exist in areas of the container that are not in contact with the freeze dryer plates, such as near the edges of the container (especially in the case of flexible containers), and / or in areas where voids or pores exist in the intermediate cake. Therefore, it is desirable to develop improved components and processes for freeze-drying / lyophilizing solutions. [Means for solving the problem]

[0008] This section provides a general overview of the disclosure and is not an exhaustive disclosure of the entire scope or all features.

[0009] In various aspects, the present disclosure provides a freeze dryer.

[0010] In at least one exemplary embodiment, a freeze dryer includes a shelf and a container, wherein at least one of the shelf and the container comprises a material having an emissivity of about 0.6 or more and about 1.0 or less.

[0011] In at least one exemplary embodiment, the shelf comprises a plate body containing the material.

[0012] In at least one exemplary embodiment, the shelf comprises a plate body and a coating disposed on one or more surfaces of the plate body, the coating including the material.

[0013] In at least one exemplary embodiment, the emissivity is a first emissivity and the plate body has a second emissivity that is less than the first emissivity.

[0014] In at least one exemplary embodiment, the emissivity is a first emissivity and the plate body has a second emissivity that is the same as the first emissivity.

[0015] In at least one exemplary embodiment, the container comprises a flexible structure and a fitting configured to receive and hold the flexible structure, the fitting including the material.

[0016] In at least one exemplary embodiment, the material is a first material, the emissivity is a first emissivity, and the shelf comprises a plate body including a second material having a second emissivity, the second emissivity being between about 0.6 and about 1.0.

[0017] In at least one exemplary embodiment, the material is a first material, the emissivity is a first emissivity, the shelf comprises a plate body and a coating disposed on one or more surfaces of the plate body, the coating comprising a second material having a second emissivity, the second emissivity being between about 0.6 and about 1.0.

[0018] In at least one exemplary embodiment, the emissivity is greater than or equal to about 0.8 and less than or equal to about 1.0.

[0019] In various aspects, the present disclosure provides a shelf plate for a freeze dryer.

[0020] In at least one exemplary embodiment, the shelf plate comprises a plate body and a material layer disposed on or comprising one or more surfaces of the plate body, the material layer having an emissivity of about 0.6 or more and about 1.0 or less.

[0021] In at least one exemplary embodiment, the emissivity is a first emissivity and the plate body has a second emissivity that is less than the first emissivity.

[0022] In at least one exemplary embodiment, the emissivity is a first emissivity and the plate body has a second emissivity that is the same as the first emissivity.

[0023] In at least one exemplary embodiment, the layer of material is a continuous coating.

[0024] In at least one exemplary embodiment, the layer of material is a discontinuous coating.

[0025] In at least one exemplary embodiment, the material layer is an anodized layer.

[0026] In at least one exemplary embodiment, the material layer comprises a fluoropolymer.

[0027] In at least one exemplary embodiment, the fluoropolymer comprises polytetrafluoroethylene.

[0028] In at least one exemplary embodiment, the plate body has at least one surface having a non-planar configuration.

[0029] In at least one exemplary embodiment, the plate assembly is configured to receive a container, the container comprising a flexible structure and a fitting configured to receive and hold the flexible structure.

[0030] In at least one exemplary embodiment, the emissivity is a first emissivity, the fixture includes one or more portions having a second emissivity, and the second emissivity is an emissivity between about 0.6 and about 1.0.

[0031] Further areas of applicability will become apparent from the description provided herein. The description and specific examples in this summary are intended for purposes of illustration only and are not intended to limit the scope of the present disclosure.

[0032] The drawings herein are for purposes of illustrating selected embodiments only, not all possible implementations, and are not intended to limit the scope of the present disclosure. [Brief explanation of the drawings]

[0033] [Figure 1] FIG. 1 is a diagram of an example of a freeze dryer including a shelf structure, in accordance with at least one exemplary embodiment of the present disclosure. [Figure 2] FIG. 2 is a diagram of another example of a freeze dryer including a shelf structure, in accordance with at least one exemplary embodiment of the present disclosure. [Figure 3] FIG. 3 is a diagram of an example shelf structure, in accordance with at least one exemplary embodiment of the present disclosure. [Figure 4A] FIG. 4A is a diagram of an example plate structure including a high emissivity material, in accordance with at least one exemplary embodiment of the present disclosure. [Figure 4B] FIG. 4B is a diagram of an example plate structure including a high-emissivity coating, in accordance with at least one exemplary embodiment of the present disclosure. [Figure 5A] FIG. 5A is a diagram of another example plate structure including a high-emissivity coating, in accordance with at least one exemplary embodiment of the present disclosure. [Figure 5B] FIG. 5B is a diagram of an example plate structure including a high-emissivity coating, in accordance with at least one exemplary embodiment of the present disclosure. DETAILED DESCRIPTION OF THE INVENTION

[0034] Corresponding reference symbols indicate corresponding parts in the above figures.

[0035] Exemplary embodiments will be described in more detail with reference to the accompanying drawings.

[0036] The exemplary embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope to those skilled in the art. Numerous specific details are set forth, such as examples of specific components, devices, and methods, to provide a thorough understanding of the embodiments of the present disclosure. It will be apparent to those skilled in the art that specific details are not necessary, that the exemplary embodiments may be embodied in many different forms, and that none of these should be construed as limiting the scope of the present disclosure. In some exemplary embodiments, well-known processes, well-known device structures, and well-known technologies are not described in detail.

[0037] The terminology used herein is for the purpose of describing particular exemplary embodiments only and is not intended to be limiting. As used herein, the singular forms "a," "an," and "the" are intended to include the plural forms unless the context clearly dictates otherwise. The terms "comprises," "comprising," "including," and "having" are inclusive and thus specify the presence of stated features, entities, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. The method steps, processes, and operations described herein should not be construed as necessarily requiring performance in the particular order described or illustrated, unless specifically identified as such. It should also be understood that additional or alternative steps may be employed.

[0038] When an element or layer is referred to as "on," "engaged to," "connected to," or "coupled to" another element or layer, it may be directly on, directly engaged with, directly connected to, or directly coupled to the other element or layer, or intervening elements or layers may be present. Conversely, when an element is referred to as "directly on," "directly engaged with," "directly connected to," or "directly coupled to" another element or layer, there are no intervening elements or layers present. Other terms used to describe relationships between elements should be interpreted similarly (e.g., "between" vs. "directly between," "adjacent" vs. "directly adjacent," etc.). As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0039] Terms such as "first," "second," and "third" may be used herein to describe various elements, components, regions, layers, and / or sections, but these elements, components, regions, layers, and / or sections should not be limited by these terms. These terms are used only to distinguish one element, component, region, layer, or section from another region, layer, or section. Terms such as "first," "second," and other numerical terms, when used herein, do not imply a sequence or order unless clearly indicated by context. Thus, a first element, first component, first region, first layer, or first section described below could also be referred to as a second element, second component, second region, second layer, or second section without departing from the teachings of the exemplary embodiments.

[0040] Spatial terms such as "inside," "outside," "beneath," "below," "lower," "upper," and "above" are used herein for ease of description when describing the relationship of one element or feature to another element(s) or feature(s), as shown in the figures. Spatial terms may be intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures were inverted, elements described as being "beneath" or "beneath" other elements or features would change accordingly to be "above" them. Thus, for example, the term "below" can encompass both an orientation of above and below. The device may be otherwise oriented (rotated 90 degrees or at other orientations), and the spatial descriptions used herein should be interpreted accordingly.

[0041] Various components are referred to herein as "operably associated." As used herein, "operably associated" refers to components that are linked together in an operable manner and includes embodiments in which components are directly coupled as well as embodiments in which other components are disposed between the coupled components. "Operably associated" components can be "fluidically associated." "Fluidly associated" refers to components that are linked together so that fluid can be transported between them. The term "fluidly associated" includes embodiments in which other members are disposed between two fluidly associated members, embodiments in which members are directly connected, and the like. Fluidly associated members may include members that do not contact the fluid but that operate the system by contacting other members (e.g., a peristaltic pump that compresses the outside of a flexible tube to pump fluid through the tube).

[0042] Exemplary embodiments will be described in more detail with reference to the accompanying drawings.

[0043] 1 illustrates an example of an apparatus 100 for freeze-drying materials in liquid, solid, or combination thereof form (including, for example, biological materials and / or food and / or pharmaceuticals) to increase the shelf life of such materials and improve the transportation and safe handling of such materials. As shown, apparatus 100 comprises a chamber 104 containing a shelving structure (also referred to as a shelving system) 112 configured to hold the material to be freeze-dried, and a housing 108 in communication with chamber 104 and including a user interface 116.

[0044] The housing 108 includes a vacuum system (not shown) configured to create a low-pressure environment within the chamber 104, a temperature control system (not shown) configured to control the temperature of the shelf structure 112, a vapor condensation system (not shown) configured to collect and retain sublimated vapors emerging from the chamber 104, and a control system (not shown) including, for example, a computer system having one or more processors for controlling various functions of the apparatus. The user interface 116 is configured to allow an operator to input data, parameters, and other information to control specific functions of the apparatus 100. For example, the user interface 116 allows an operator to communicate with the control system to create and execute custom processes for freeze-drying different substances, including programmable multi-stage cycles.

[0045] The materials to be freeze-dried may be arranged on separate shelves of the shelving structure 112. A temperature control system disposed within the housing 108 and configured to vary the temperature of the shelving structure 112 is used to first freeze the materials to be freeze-dried and then further reduce the temperature of the frozen materials to a predetermined level, e.g., the temperature to be maintained during the sublimation stage of the freeze-drying cycle. For example, in the case of water sublimation, the temperature is selected to be below the triple point, useful for preserving materials suspended or dissolved in aqueous solutions. For example, in at least one exemplary embodiment, the predetermined level is a temperature of about −30° C. or higher to about −20° C. or lower.

[0046] After the material to be freeze-dried is frozen and further cooled to a predetermined temperature, a vacuum system disposed within the housing 108 and configured to vary the pressure within the chamber 104 is used to create a pressure below atmospheric pressure within the chamber 104. For example, in at least one exemplary embodiment, the pressure is reduced to and maintained at less than about 100 mTorr absolute for a sublimation period. The sublimation phase or period is the time period from the start of sublimation to the end of sublimation. Sublimation begins when the pressure and temperature within the chamber 104 are below the triple point of the chamber environment. Sublimation ends when all ice has been removed from the material to be freeze-dried. The sublimation period varies depending on the material to be freeze-dried, the amount of material to be freeze-dried, and the shape, e.g., thickness, of the material to be freeze-dried.

[0047] In at least one exemplary embodiment, the vacuum system cooperates with a vapor condensing system to maintain the environment within chamber 104 at a pressure lower than atmospheric pressure. Because sublimation occurs at a low chamber pressure, escaping vapor can carry heat energy away from the material to be freeze-dried. The escaping vapor is then captured in the vapor condensing system contained within housing 108. Continuous capture of sublimated vapor by the vapor condensing system helps maintain a low chamber pressure within sublimation chamber 104. A control system within housing 108 is programmed to control the temperature of shelf structure 112 so that the shelf structure is maintained at a temperature sufficient to compensate for escaping heat energy and maintain sublimation until all volatile material has been removed from the material to be freeze-dried (i.e., the end of the sublimation period). After sublimation of essentially all volatile and / or other material components (i.e., the end of the sublimation period), the shelf temperature setting is increased and maintained at that temperature for an additional period to desorb one or more other material components from the material to be freeze-dried. The one or more other material components may be components previously adsorbed or absorbed by the material to be freeze-dried. After desorption is complete, the pressure in the chamber is returned to atmospheric pressure and the completely dried product is collected.

[0048] 2 illustrates another example of an apparatus 200 for freeze-drying materials in liquid, solid, or combination thereof form (including, for example, biological materials and / or food and / or pharmaceuticals) to increase the shelf life of such materials and to improve the transportation and safe handling of the materials. Apparatus 200 is similar to apparatus 100, except that in apparatus 200, chamber 204 is disposed within housing 208. Like chamber 104, chamber 204 is configured to include a shelving structure (or shelving system) 212 configured to hold the material to be freeze-dried. Also, like housing 108, housing 208 includes a user interface 216 configured to allow an operator to input data, parameters, and other information to control certain functions of apparatus 200.

[0049] Figure 3 shows an example of a shelving structure 320 that can be used for various freeze-drying processes, including the shelving structures 112, 212 for the freeze-dryers 100, 200 shown in Figures 1 and 2. The shelving structure 320 includes a plurality of plates 304 that extend between and are movable along a pair of side rails 322, 324. Each plate 304 defines a surface 326 for placement of the material to be freeze-dried. In some variations, depending on the type of material to be freeze-dried, the material is held in a container 328 (such as a fixture, tray, bag, or bottle). The container 328 is positioned on the plate 304 as shown. The container 328 may be similar to those described in U.S. Pat. No. 11,747,082 ("Multi-Part Freeze-Drying Container and Method of Use Thereof," issued September 5, 2023, inventors: Kestas P. Parakininkas, Eric T. Hansen, Kirk L. Weimer, Nathaniel T. Johnson, and Dennis J. Hlavinka) and / or U.S. Pat. No. 11,609,042 ("Multi-Part Freeze-Drying Container and Method of Use Thereof," issued March 21, 2023, inventors: Kestas P. Parakininkas, Eric T. Hansen, Kirk L. Weimer, Nathaniel T. Johnson, and Dennis J. Hlavinka) and / or U.S. Pat. No. 10,793,327 ("Freeze-Drying Container and Method of Use Thereof," issued October 6, 2022, inventors: Kirk No. 11,634,257 ("Freeze-Drying Container and Method of Use Thereof," issued April 25, 2023, inventors: Kirk L. Weimer, Nate T. Johnson, Dennis J. Hlavinka, and Kestas P. Parakininkas), the entire disclosures of which are incorporated herein by reference.

[0050] For example, in at least one exemplary embodiment, the container 328 is a generally flexible container, such as a bag and / or tray, that does not evenly contact the plates 304, 308. In other exemplary embodiments, the container 328 includes a fitting configured to receive a bag or other generally flexible structure that carries or holds the material to be freeze-dried. In such cases, the fitting is sized to receive, house, and confine the bag or other flexible structure throughout the freeze-drying process. In at least one exemplary embodiment, the fitting includes one or more seal structures configured to hold the bag or other flexible structure within the fitting. In at least one exemplary embodiment, the fitting is configured to receive an empty bag or other flexible structure, and after the bag or other flexible structure is received and positioned, the material to be freeze-dried is added to the bag or other flexible structure. A gas, such as air or carbon dioxide, is then introduced into the bag or other flexible structure, causing the bag or other flexible structure to conform to the dimensions of the fitting. The assembly (including the fitting, the bag or other flexible structure containing the material to be freeze-dried, and (optionally) the gas) is subjected to a freeze-drying cycle as detailed above. In at least one exemplary embodiment, one or more seal structures are adjusted during the freeze-drying cycle to allow vapor escape.

[0051] As shown in FIG. 3 , in at least one exemplary embodiment, the shelving structure 320 further includes an end plate 308 that is parallel to the plates 304 and extends between the pair of rails 322, 324. The end plate 308 may be a fixed plate. The shelving structure 320 includes a motion control system 312 configured to vary the distance between the plates 304. For example, varying the distance between the plates 304 interacts with the container 328 during the freeze-drying process. In at least one exemplary embodiment, interacting with the container 328 includes, for example, closing the container 328 upon completion of the freeze-drying process. The motion control system 312 includes various components that cooperate to move the plates 304. For example, in at least one exemplary embodiment, the motion control system 312 includes a computer system that includes memory, input devices, output devices, communication devices, and / or subsystems such as a hydraulic system, a pneumatic system, or a mechanical system that includes one or more motors, actuators, pumps, compressors, cylinders, pistons, tubing, valves, bladders, sensors, and / or regulators. The movement control system 312 is removably coupled to the plate 304 using any suitable connections, including, for example, connectors, tubing, fittings, tubes, and / or adapters.

[0052] The shelving structure 320 includes a thermal fluid system 316 configured to circulate a thermal fluid through and / or around at least a portion of the plurality of plates 304. For example, in at least one exemplary embodiment, the thermal fluid system 316 is removably coupled to the plates 304 using any suitable connections including, for example, connectors, tubing, fittings, tubes, and / or adapters. In each instance, the movement of the thermal fluid removes energy from and / or adds energy to at least a portion of the plurality of plates 304. For example, the movement of the thermal fluid controls the temperature of one or more of the plurality of plates and the temperature of the material to be freeze-dried disposed on the plates.

[0053] In each variation, one or more of the plurality of plates 304 and / or end plates 308 and / or vessel 328 (particularly if vessel 328 includes a fixture) includes (e.g., is formed from) or is (at least partially) coated with a high emissivity material (e.g., a material having an emissivity greater than about 0.9), for example, to help maintain the temperature of the plurality of plates 304 and / or end plates 308 and / or vessel 328 above ice temperature.

[0054] All objects emit thermal radiation at temperatures above absolute zero. For example, the emissivity of an object is the relative ability of its surface to release heat by radiation. Emissivity can be defined as the ratio of the energy radiated from the surface of an object to the energy radiated from an ideal radiator (e.g., a black body) at the same temperature. Emissivity values ​​are dimensionless and range from 0 to 1, where a black body (e.g., a perfect radiator) has an emissivity of 1 and a perfect reflector has an emissivity of 0. Incorporating high-emissivity materials in freeze-drying applications can increase radiative heat transfer and more easily heat materials not in contact with the freeze-dryer plates (e.g., intermediate cakes) (e.g., as a result of cake buckling and / or raised edges (especially in the case of flexible containers)).

[0055] In at least one exemplary embodiment, one or more of the plurality of plates 304 and / or end plates 308 and / or enclosure 328 (particularly if enclosure 328 includes a fixture) include (e.g., are formed from) a high emissivity material. For example, one or more of the plurality of plates 304 and / or end plates 308 and / or enclosure 328 (particularly if enclosure 328 includes a fixture) include a material having an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater.

[0056] In at least one exemplary embodiment, one or more of the plurality of plates 304 and / or end plates 308 and / or container 328 (particularly if container 328 includes fixtures) comprise (e.g., are formed of) a metallic material including, for example, aluminum, stainless steel, steel, iron, copper, titanium, brass, nickel, or any combination thereof. In at least one exemplary embodiment, one or more of the plurality of plates 304 and / or end plates 308 and / or container 328 (particularly if container 328 includes fixtures) comprise (e.g., are formed of) aluminum having a polished surface with an emissivity of about 0.04 or more to about 0.06 or less and / or stainless steel having a polished surface with an emissivity of about 0.075. In at least one exemplary embodiment, polished stainless steel is preferred due to its corrosion resistance and its resistance to very aggressive cleaning agents, particularly required for food or medical applications.

[0057] In at least one exemplary embodiment, one or more of the plurality of plates 304 and / or end plates 308 and / or enclosure 328 (particularly if the enclosure 328 includes a fixture) includes (e.g., is formed from) a first material having a first emissivity and is coated (at least partially) with a second material having a second emissivity greater than the first emissivity. The second material forming the coating has an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. In at least one exemplary embodiment, the first material includes a metallic material, and the second material includes various oil-based paints having an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. In at least one exemplary embodiment, the first material includes, for example, polished aluminum having an emissivity of about 0.04 or greater to about 0.06 or less, and / or polished stainless steel having an emissivity of about 0.075. In at least one exemplary embodiment, the second material includes an optical black paint, such as 3M's Black Velvet Coating 9560 series. In at least one exemplary embodiment, the second material includes a fluoropolymer, such as polytetrafluoroethylene, having an emissivity greater than about 0.9. In yet other exemplary embodiments, for example, when the first material is aluminum, the second material includes an anodized layer produced using an electrochemical surface treatment process. In each case, the coating has a thickness sufficient to increase the emissivity to greater than about 0.9. One or more of the plurality of plates 304 and / or end plates 308 and / or container 328 (especially if the container 328 includes a fixture) having a high-emissivity coating has an emissivity of about 0.9 or greater to about 1 or less.

[0058] 4A and 4B illustrate a plate structure 700 that can be used in various freeze-drying processes, including plates such as plates 304, 308 of shelf structure 320 shown in FIG. 2. Plate structure 700 illustrates two plates: a first plate 704 and a second plate 708. First plate 704 has a surface 712 that faces a surface 716 of second plate 708. A space 720 is defined between surface 712 of the first plate and surface 716 of second plate 708. A container 740 configured to carry (or hold) a material 760 to be freeze-dried is disposed within space 720. In at least one exemplary embodiment, container 740 comprises a flexible container that does not uniformly contact plate 708. In other exemplary embodiments, container 740 comprises a fitting configured to receive a bag or other flexible structure that carries or holds the material to be freeze-dried. The first plate 704 and the second plate 708 have similar structures. For example, in at least one exemplary embodiment, as shown, the first plate 704 has a plurality of channels 724 configured to provide a flow path for a thermal fluid used to control the temperature of the first plate 704. Similarly, the second plate 708 has a plurality of channels 744 configured to provide a flow path for a thermal fluid used to control the temperature of the second plate 708.

[0059] In each example, first plate 704 and / or second plate 708 and / or container 740 (particularly in examples in which container 740 includes a fixture) includes (e.g., is formed from) or is coated (at least partially) with a high-emissivity material (e.g., a material having an emissivity greater than about 0.9).

[0060] 4A, the first plate 704 and / or the second plate 708 include (e.g., are formed from) a high emissivity material. For example, the first plate 704 and / or the second plate 708 include a material having an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater.

[0061] 4B , the first plate 704 and / or the second plate 708 include (e.g., are formed of) a first material having a first emissivity and are coated (at least partially) with a second material having a second emissivity greater than the first emissivity. The second emissivity may be about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. The second material may coat one or more surfaces of the first plate 704 and / or the second plate 708 to form one or more high-emissivity coatings 750. The high-emissivity coating 750 includes one or more layers and may be, for example, a discontinuous or substantially continuous coating covering about 75% or more, optionally about 80% or more, optionally about 85% or more, optionally about 90% or more, optionally about 95% or more, optionally about 98% or more, optionally about 99% or more, and in certain embodiments, optionally about 99.5% or more of the total surface area of ​​one or more surfaces of the first plate 704 and / or second plate 708. In other exemplary embodiments, the high-emissivity coating may be a continuous coating covering, for example, about 75% or more, optionally about 80% or more, optionally about 85% or more, optionally about 90% or more, optionally about 95% or more, optionally about 98% or more, optionally about 99% or more, and in certain aspects, optionally about 99.5% or more of the total surface area of ​​the plates 704, 708 aligned with (e.g., in contact with) the container (e.g., tray, bag, or bottle) containing the material to be freeze-dried. In each case, the coating 750 should be of sufficient continuity and thickness to provide an emissivity of the shelf surface greater than about 0.9. One or more of the first plate 704 and / or second plate 708 that includes (e.g., is formed from) a high-emissivity material has an emissivity of about 0.9 or more to about 1 or less.

[0062] In at least one exemplary embodiment, the first material includes a metallic material, and the second material includes various oil-based paints having an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. In at least one exemplary embodiment, the first material includes, for example, polished aluminum having an emissivity of about 0.04 or greater to about 0.06 or less, and / or polished stainless steel having an emissivity of about 0.075. In at least one exemplary embodiment, the second material includes, for example, optical black paint from 3M's Black Velvet Coating 9560 series. In at least one exemplary embodiment, the second material includes a fluoropolymer, such as polytetrafluoroethylene, having an emissivity greater than about 0.9. In yet another exemplary embodiment, for example, when the first material is aluminum, the second material includes an anodized layer produced using an electrochemical surface treatment process. In each case, the coating has a thickness sufficient to increase the emissivity to greater than about 0.9. One or more of the first plate 704 and / or second plate 708 that include a high-emissivity coating have an emissivity of about 0.9 or more to about 1 or less.

[0063] 5A and 5B show another plate structure 900 that can be used in various freeze-drying processes, including plates such as plates 304, 308 of shelf structure 320 shown in FIG. 3. The illustrated plate structure 900 shows two exemplary plates: a first plate 904 and a second plate 908. The first plate 904 includes a first surface 912 that faces a second surface 916 of the second plate 908. A space 920 is defined between the surface 912 of the first plate and the surface 916 of the second plate 908. A container 940 configured to carry (or hold) a material 960 to be freeze-dried is disposed within the space 920. In at least one exemplary embodiment, the container 940 is a flexible container that does not uniformly contact the plate 908. In other exemplary embodiments, the container 940 includes a fitting configured to receive a bag or other flexible structure that carries or holds the material to be freeze-dried.

[0064] In at least one exemplary embodiment, the plate surface away from the vessel 940, such as the first surface 912 of the first plate 904 as shown, is shaped to increase the overall surface area and thereby increase radiation from the first surface 912. For example, as shown, the plate surface away from the vessel 940, such as the first surface 912 of the first plate 904, has a non-planar (e.g., wavy) configuration. However, it should be recognized that in other variations, other geometric configurations can be selected to increase and thereby improve the radiation surface area. The first plate 904 and the second plate 908 have similar structures. For example, in at least one exemplary embodiment, as shown, the plate 904 has a plurality of channels 924 configured to provide a flow path for a thermal fluid used to control the temperature of the first plate 904. Similarly, the second plate 908 has a plurality of channels 944 configured to provide a flow path for a thermal fluid used to control the temperature of the second plate 908.

[0065] In each example, first plate 904 and / or second plate 908 and / or container 940 (particularly in examples in which container 940 includes a fixture) includes (e.g., is formed from) or is coated (at least partially) with a high-emissivity material (e.g., a material having an emissivity greater than about 0.9).

[0066] 5A , the first plate 904 and / or the second plate 908 include (e.g., are formed from) a high-emissivity material. For example, the first plate 904 and / or the second plate 908 include a material having an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. One or more of the first plate 904 and / or the second plate 908 that include (e.g., are formed from) a high-emissivity material have an emissivity of about 0.9 or greater to about 1 or less.

[0067] In other exemplary embodiments, for example, as shown in FIG. 5B , the first plate 904 and / or the second plate 908 include (e.g., are formed of) a first material having a first emissivity and are coated (at least partially) with a second material having a second emissivity greater than the first emissivity. The second emissivity may be about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. The second material may coat one or more surfaces of the first plate 904 and / or the second plate 908 to form one or more high-emissivity coatings 950. The high-emissivity coating 950 includes one or more layers and may be, for example, a discontinuous or substantially continuous coating covering about 75% or more, optionally about 80% or more, optionally about 85% or more, optionally about 90% or more, optionally about 95% or more, optionally about 98% or more, optionally about 99% or more, and in certain embodiments, optionally about 99.5% or more of the total surface area of ​​one or more surfaces of the first plate 904 and / or second plate 908. In other exemplary embodiments, the high-emissivity coating 950 may be a continuous coating covering, for example, about 75% or more, optionally about 80% or more, optionally about 85% or more, optionally about 90% or more, optionally about 95% or more, optionally about 98% or more, optionally about 99% or more, and in certain aspects, optionally about 99.5% or more of the total surface area of ​​the portions of the plates 904, 908 that are aligned with (e.g., in contact with) the containers (such as trays, bags, or bottles) containing the material to be freeze-dried. In each case, the high-emissivity coating 950 should be of sufficient continuity and thickness to increase the shelf surface emissivity to greater than about 0.9.

[0068] In at least one exemplary embodiment, the first material includes a metallic material, and the second material includes various oil-based paints having an emissivity of about 0.6 or greater, optionally about 0.8 or greater, and in certain aspects, optionally about 0.9 or greater. In at least one exemplary embodiment, the first material includes, for example, polished aluminum having an emissivity of about 0.04 or greater to about 0.06 or less, and / or polished stainless steel having an emissivity of about 0.075. In at least one exemplary embodiment, the second material includes, for example, optical black paint from 3M's Black Velvet Coating 9560 series. In at least one exemplary embodiment, the second material includes a fluoropolymer, such as polytetrafluoroethylene, having an emissivity greater than about 0.9. In yet another exemplary embodiment, for example, when the first material is aluminum, the second material includes an anodized layer produced using an electrochemical surface treatment process. In each case, the coating has a thickness sufficient to increase the emissivity to greater than about 0.9. One or more of the first plate 904 and / or second plate 908 that include a high-emissivity coating have an emissivity of about 0.9 or more to about 1 or less.

[0069] Although not specifically shown, it should be appreciated that in various aspects, freeze dryers 100, 200 and / or shelf structures 320 and / or plate structures 700, 900 can include various other components. For example, in at least one exemplary embodiment, freeze dryers 100, 200 and / or shelf structures 320 and / or plate structures 700, 900 can include various plate structures and / or components and / or mechanisms for moving plates, such as those described in U.S. Pat. No. 10,969,171 ("Freeze Drying," issued April 6, 2021, inventors: Frank Corbin III, Dennis J. Hlavinka, Rajesh Pareta, and Mark E. Hillam) and / or U.S. Pat. No. 11,067,336 ("Freeze Drying," issued July 20, 2021, inventors: Frank Corbin III, Dennis J. Hlavinka, Rajesh Pareta, and Mark E. Hillam). The entirety of the above-referenced US patent application is expressly incorporated herein by reference.

[0070] The foregoing description of the embodiments has been provided for purposes of illustration and description. It is not intended to be exhaustive or to limit the present disclosure. Individual elements or features of a particular embodiment are generally not limited to that particular embodiment and, even if not specifically shown or described, may be interchangeable and used in selected embodiments, where applicable. The same may be modified in many ways. Such modifications should not be considered a departure from the present disclosure, and all such variations are intended to be included within the scope of the present disclosure.

Claims

1. A freeze-dryer comprising: Shelves and A container and Equipped with At least one of the shelf and the container comprises a material having an emissivity of about 0.6 or more and about 1.0 or less. Freeze dryer.

2. The freeze dryer according to claim 1, The shelf includes a plate body containing the material. Freeze dryer.

3. The freeze dryer according to claim 1, The shelf is A plate body; a coating disposed on one or more surfaces of the plate body; Equipped with The coating comprises the material. Freeze dryer.

4. The freeze dryer according to claim 3, the emissivity is a first emissivity; the plate body has a second emissivity that is less than the first emissivity; Freeze dryer.

5. The freeze dryer according to claim 3, the emissivity is a first emissivity; the plate body has a second emissivity that is the same as the first emissivity; Freeze dryer.

6. The freeze dryer according to claim 1, The container comprises: a flexible structure; a fixture configured to receive and hold the flexible structure; Equipped with The fixture comprises the material. Freeze dryer.

7. The freeze dryer according to claim 6, the material is a first material; the emissivity is a first emissivity; the shelf comprises a plate body including a second material having a second emissivity, the second emissivity being between about 0.6 and about 1.0; Freeze dryer.

8. The freeze dryer according to claim 6, the material is a first material; the emissivity is a first emissivity; The shelf is A plate body; a coating disposed on one or more surfaces of the plate body; Equipped with the coating includes a second material having a second emissivity, the second emissivity being greater than or equal to about 0.6 and less than or equal to about 1.0; Freeze dryer.

9. The freeze dryer according to claim 1, the emissivity is greater than or equal to about 0.8 and less than or equal to about 1.0; Freeze dryer.

10. 1. A shelf plate for a freeze dryer, the shelf plate comprising: A plate body; a layer of material disposed on or constituting one or more surfaces of the plate; Equipped with the material layer has an emissivity of about 0.6 or more and about 1.0 or less; Shelf plate.

11. 11. The shelf plate of claim 10, the emissivity is a first emissivity; the plate body has a second emissivity that is less than the first emissivity; Shelf plate.

12. 11. The shelf plate of claim 10, the emissivity is a first emissivity; the plate body has a second emissivity that is the same as the first emissivity; Shelf plate.

13. 11. The shelf plate of claim 10, the layer of material is a continuous coating; Shelf plate.

14. 11. The shelf plate of claim 10, the material layer is a discontinuous coating; Shelf plate.

15. 11. The shelf plate of claim 10, the material layer is an anodized layer; Shelf plate.

16. 11. The shelf plate of claim 10, the material layer comprises a fluoropolymer; Shelf plate.

17. 17. The shelf plate of claim 16, The fluoropolymer comprises polytetrafluoroethylene. Shelf plate.

18. 11. The shelf plate of claim 10, The plate body has at least one surface having a non-planar configuration. Shelf plate.

19. 11. The shelf plate of claim 10, the plate body is configured to receive a container; The container comprises: a flexible structure; a fixture configured to receive and hold the flexible structure; Equipped with Shelf plate.

20. 20. The shelf plate of claim 19, the emissivity is a first emissivity; the fixture includes one or more portions having a second emissivity, the second emissivity being an emissivity of greater than or equal to about 0.6 and less than or equal to about 1.0; Shelf plate.

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