Microwave lyophilizer having corona discharge control

Information

  • Patent Grant
  • 6225611
  • Patent Number
    6,225,611
  • Date Filed
    Monday, November 15, 1999
    25 years ago
  • Date Issued
    Tuesday, May 1, 2001
    23 years ago
Abstract
A lyophilizer system is adapted for operation in a first mode or a second mode with microwave assisted drying. The system includes a lyophilizing chamber, including shielding from microwaves. The chamber is connected to a pressure controller for controlling vacuum in the lyophilizing chamber and a device for trapping water vapor. One or more microwave generators, direct microwaves into the lyophilizing chamber. Refrigeration units lower the temperature of the lyophilizing chamber and condenser. The chamber environment maintains a temperature and a pressure that facilitates sublimation in the chamber in a first mode, and for creating a chamber environment having vacuum and temperature such that when combined with microwaves directed into the chamber, facilitates sublimation in the chamber in a second mode. The chamber has arc inhibiting surfaces and shielding and a corona discharge detection and control system, including optical, thermal and other detection systems.
Description




BACKGROUND OF THE INVENTION




1. Field of the Invention




The present invention is directed to an improved system for lyophilizing with microwaves and an improved method for microwave lyophilization.




2. Prior Art




Lyophilization, or freeze drying, as it is more commonly known, is used in a number of different industries to remove water from materials to achieve a more stable pure product with a prolonged shelf life. The process is used in the pharmaceutical and food industries which require lyophilization systems that are capable of producing environmental processing conditions to effect sublimation so that the water is removed from processed materials. The water vapor is drawn off from the lyophilization chamber and typically removed by trapping on a refrigerated condenser surface, desiccants or other suitable devices.




Sublimation is a process wherein materials change from a solid phase directly to a gaseous phase without passing through a liquid phase. With water, ice turns directly to water vapor without first melting to a liquid form, and then evaporating. Sublimation can occur at various temperatures and pressure combinations, but typically sublimation needs low temperatures and a vacuum pressure less than atmospheric. Sublimation provides advantages for materials processing as purity is maintained and the processed material does not have to be subjected to high temperatures, such as would be needed to boil off the water.




Although traditional lyophilization systems have worked well for their intended purpose, they have several shortcomings. Traditional lyophilization systems must attain subzero temperatures and create vacuum conditions to provide atmospheric processing conditions that facilitate sublimation. These types of lyophilization systems have shortcomings that lessen their usefulness. Such systems require large amounts of energy for refrigeration equipment, for creating and maintaining the vacuum, and for providing the heat, primarily through convection and conduction, for sublimating the ice and warming the product and the system. In addition, to compound the high energy consumption, such traditional lyophilization processes are very time consuming. Often, the freeze drying may take a week or more, creating a bottleneck in the material processing. To accommodate high production needs, the size of the freeze drying systems must be quite large to handle large batches. Furthermore, should problems develop during the freeze drying process, large batches of material may be damaged. As the systems require large amounts of energy to maintain the atmospheric conditions for an extended period of time, the operating costs are high, thereby increasing the total cost of processing the product.




To increase the speed of the drying process and to decrease the amount of energy required for heating, including energy necessary to heat the mass of shelving for radiation, convection and conductive heating of the material to be processed, systems and methods have been developed that use microwaves to aid freeze drying. Although for freeze drying, such systems still require vacuum and a condenser or other system for collecting the liberated water vapor, the energy needed to maintain temperatures for sublimation is decreased as microwaves are used in the sublimation process. Such systems achieve freeze drying of the materials, but do so in greatly reduced time periods. Processing taking several days or a week or more with conventional lyophilization may now be performed in less than a day, and in many cases, several hours. The microwaves provide the energy of sublimation directly to the materials being processed, alone or in combination with radiation, convection and/or conduction, so that sublimation occurs much more efficiently.




Though microwaves have been used to speed the freeze drying process, and are successful when operated and controlled correctly, there are problems associated with such systems. Prior microwave systems operating under vacuum conditions suffer from uncontrollable corona discharge, which occurs when high electric fields ionize gases within the freeze drying chamber. Sharp edges of metallic objects can enhance the local electric field and ignite gases and create a corona discharge. Such occurrences of corona discharge create localized temperature spikes that may cause localized overheating or melting, adversely affecting the materials near the occurrence. This affects the quality of the freeze dried product, since many products, including many pharmaceutical and biological products are temperature sensitive, have very high quality standards. Corona discharge can be fatal to the success of the freeze drying process. Non-uniform microwave coverage can also adversely affect the quality of the product being processed.




Heretofore, prior art microwave systems have not employed a method of successfully reducing or eliminating corona discharge within the freeze drying chamber. Moreover, such systems have not employed detectors to sense when corona discharges occur. Even if they had detected problems, such systems do not have controls to adjust conditions in response to detected arcing in order to minimize or eliminate the occurrences of corona discharge in time to reduce damage to the product.




Examples of freeze drying apparatuses using microwaves to assist in drying are shown in U.S. Pat. Nos. 2,859,534 and 3,020,645 to Copson, and U.S. Pat. NO. 3,048,928 to Copson et al. Although the Copson patents teach microwave friendly trays to limit discharge in the processing chamber, and removing condensation coils from the inner processing container, no additional steps are shown or suggested to actively control and monitor microwave discharge. U.S. Pat. No. 3,264,747 to Fuentevilla teaches a microwave assisted freeze drying apparatus using non-conductive materials such as Plexiglas to contain the product. Although microwaves are utilized, there is no system for detection, control, and/or elimination of corona discharge.




A major hurdle with detection systems is that temperature sensors typically are made of materials that, if extended into the microwave field, would create further discharges. Therefore, traditional temperature, pressure, and other sensors to be placed within the microwave field often cannot be utilized without modification.




It can be seen then that a need exists for a new and improved system for microwave assisted lyophilization. Such a system should greatly reduce the time and energy required to uniformly freeze dry the material being processed. In addition, such a system utilizing microwave energy should be configured to minimize the potential effects of corona discharge within the lyophilization chamber. The system should provide microwave distribution to all materials placed in the chamber and provide relatively uniform processing of the materials in the chamber. Such a lyophilization system should also utilize detectors and controls to detect the occurrence of actual and/or incipient corona discharges and to adjust the microwave field strength and other system characteristics to promptly eliminate corona discharges when detected. The present invention addresses these as well as other problems associated with microwave lyophilization systems.




SUMMARY OF THE INVENTION




The present invention is directed to a microwave assisted lyophilization system and a method for lyophilizing using microwaves. The present invention provides a lyophilization chamber that is capable of creating pressures and low temperatures sufficient to create atmospheric conditions that are conducive to sublimation, and therefore lyophilization of the product. Such freeze drying may take extended periods, often several days, a week or more. In addition, the present invention may also be operated in a mode in which microwaves are introduced into the chamber to conductively heat the containers, which then add heat to the material being processed.




The present invention includes a lyophilization system capable of withstanding suitable ranges of pressure and temperature. The system must be capable of withstanding absolute pressures as low or lower than 1 mm Hg, and for many applications, pressures required for steam sterilization of the chamber. During lyophilization, temperatures in the system may range from highs above room temperature and lows below zero centigrade. In addition to the processing chamber, all components linked by air passages to the processing chamber must also be able to withstand the vacuum and/or pressure conditions. A conductive conduit generally extends from the chamber to a vapor trap, such as condenser or similar device, for trapping the water vapor from the product being dried. The water vapor may be generated in the lyophilization chamber, and passed into the condenser, where it is generally collected as ice. The refrigeration unit is in communication with the condenser and/or lyophilization chamber to create the low temperature conditions that are necessary for lyophilization.




In addition to the refrigeration system, a vacuum pump is in communication with the chamber and condenser to place the lyophilization chamber and condenser under vacuum for the lyophilization process. The lyophilization chamber and condenser contain sensors to monitor and/or control the various conditions such as temperature and pressure levels.




In a preferred embodiment, the various sensors and the cooling and vacuum units are connected to a central controller or processor to provide displays for monitoring, adjusting and optimizing the various characteristics for the most efficient and highest quality processing.




In addition to the vacuum and temperature conditions that facilitate removal of the water content from the product, microwaves may be utilized to facilitate sublimation and therefore drying of the product. The present invention uses one or more microwave generators to expose the contents of the lyophilization chamber to microwaves while under the preferred environmental conditions that also facilitate lyophilization.




The number and power level of the microwave generators may be varied depending on the requirements of the lyophilization system and the design and capacity of the chamber. However, it is important that the entire product area in the chamber have exposure to the microwave field so that lyophilization occurs substantially uniformly throughout the product being processed. Therefore, wave guides direct the microwaves toward the chamber at various angles and spacing to facilitate substantially uniform distribution of microwaves. For a given total microwave power level, the use of multiple generators or multiple wave guide openings lowers the electrical field strength at each opening, thereby lowering the likelihood of corona discharge. In addition, stirrers may be placed in the processing chamber to distribute microwaves and provide more nearly uniform levels of microwave energy throughout the product and improve processing quality. The microwave generators are also controlled by a central processor and may be manually or automatically adjusted depending on the desired processing of the product and the various temperatures and other conditions monitored and controlled during the processing.




According to the present invention, sealed wave guide windows are placed within the wave guides. Such windows are typically made from a material such as TeflonĀ® that allows microwaves to pass through the window, while maintaining the pressure differentials across the windows. The windows have a pressure seal that withstands the vacuum and/or pressures created in the lyophilization processing chamber.




In addition to the problems created by the temperature and pressure ranges, the processing chamber encounters special problems from its exposure to microwaves. A common problem that occurs with microwaves is corona discharge, which may prevent speedy and high quality lyophilization and which has limited the commercial use of microwaves for lyophilization. To accommodate the microwaves, the processing chamber must be free of corona discharge base points, such as sharp metal edges or points. It has been found that metallic objects may be placed in the chamber as long as they do not provide such sharp edges and points that provide the base for an arc. As long as the various metallic objects are either shielded or rounded, the possibility of arcing and corona discharge occurring is greatly reduced. Therefore, the stirrer components, such as the stirrer drive shafts, are shielded and exposed surfaces are rounded. Any sensors placed within the chamber must be compatible with the microwave conditions. Temperature sensors and other sensors in the chamber must use fiber optic materials or the sensors must be shielded or remote from the microwave field. By using arc inhibiting surfaces, microwaves may be used effectively without causing corona discharge.




In addition to creating a lyophilization chamber that hinders formation of arcs, the present invention includes controls that monitor and detect corona discharge and allow for modifying chamber conditions to stop discharge from occurring. Various temperature sensors and/or photo detectors may be placed within the chambers. Should a corona discharge occur, there will be illumination and a local temperature spike. If sufficient sensors are placed in a spaced apart relationship throughout the chamber to form a sensor field, the location of such corona discharges can be determined. Incipient corona discharge can be monitored by measuring electric field strength and/or reflected power. If the location of discharges can be pinpointed, adjustments may be made in the power levels of one or more of the microwave generators and/or chamber atmospheric conditions, such as pressure and temperature, may be changed to eliminate further corona discharge. In addition to the sensors throughout the chamber, sensors may be placed proximate the wave guide windows so that arcing may be detected by the temperature sensors at each associated microwave generator. With monitoring and control available, the occurrence of corona discharge can be minimized and/or eliminated so that higher quality processing occurs and the products produced reflect that quality. In addition, as information on the conditions present to create a discharge is accumulated, processing conditions can be initialized and controlled based on accumulated processing information so that corona discharge free lyophilization may be achieved.




These features of novelty and various other advantages which characterize the invention are pointed out with particularity in the claims annexed hereto and forming a part hereof. However, for a better understanding of the invention, its advantages, and the objects obtained by its use, reference should be made to the drawings which form a further part hereof, and to the accompanying descriptive matter, in which there is illustrated and described a preferred embodiment of the present invention.











BRIEF DESCRIPTION OF THE DRAWINGS




Referring now to the drawings, wherein like reference letters and numerals indicate corresponding structure throughout the several views:





FIG. 1

shows a diagrammatic partial sectional view of a microwave lyophilizing system and associated atmospheric equipment according to the principles of the present invention;





FIG. 2

shows a top plan view of the microwave lyophilizing system shown in

FIG. 1

;





FIG. 3

shows an end sectional view of a lyophilizer chamber for the microwave lyophilization system shown in

FIG. 1

;





FIG. 4

shows a flow chart for controlling the lyophilization process of the microwave lyophilization system shown in

FIG. 1

, such as used for processing material held in vials or other sealable containers;





FIG. 5

shows a perspective view of a microwave stirrer for the lyophilization shown in

FIG. 1

;





FIG. 6

shows a elevational view of a sensor for the lyophilization system shown in

FIG. 1

;





FIG. 7

shows a perspective view of a wave guide window for the lyophilization system shown in

FIG. 1

;





FIG. 8

shows a side sectional view of a wave guide and connection to the microwave chamber; and





FIG. 9

shows an end sectional view of a lyophilizer chamber for the microwave lyophilization system shown in

FIG. 1

with a sensor cluster.











DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS




Referring now to the drawings, and in particular to

FIGS. 1 and 2

, there is shown a microwave lyophilization system, generally designated


20


. The lyophilization system


20


may be utilized as a conventional freeze drying system wherein the moisture is removed by creating atmospheric conditions that facilitate removal of the water content from the product. The atmospheric conditions include placing the system under vacuum and controlling the temperature so that direct sublimation occurs and ice changes directly to water vapor. The lyophilization system


20


includes a processing chamber


22


wherein the freeze drying process occurs. The chamber


22


includes a door


92


with monitoring window


90


formed therein. The door


92


preferably attaches to the chamber forming an opening to the full width of the chamber so that full width trays and material supported thereon may be easily inserted. The chamber


20


is preferably sealed to the door


92


with gaskets or other pressure seal devices to accommodate vacuum and pressure conditions. The chamber


20


should be capable of withstanding pressures as low or lower than 1 mm Hg, ranging to absolute pressures of several pounds per square inch.




As shown in

FIG. 3

, the lyophilization processing chamber


22


also includes shelves


60


spaced apart within the chamber


22


to support the trays or vials containing material which is to be freeze dried. In one embodiment, the processing chamber


22


is substantially cylindrical so that greater pressure variations may occur in utilizing the inherent strength properties of a rounded geometry. However, other chamber configurations, such as rectangular, may be used. Shelf supports


62


may be molded or fastened to the walls of the chamber


22


to provide for easy removal and insertion of the product and trays.




As shown in

FIGS. 1 and 2

, to accommodate the removal of water vapor from the chamber


22


, a condenser


24


or other vapor trap, such as a desiccant or similar device, is utilized. A fan


54


may be provided to facilitate circulation of air through the condenser


24


and back to the processing chamber


22


. The fan


54


serves to lower the product chamber temperature, and in some cases, to freeze the material to be lyophilized. The air or other gases, may be recirculated by suitable pipes or ducts, providing a faster method for freeze drying the material being processed. Vacuum lines including isolation valves


36


connect the condenser


24


and processing chamber


22


to a vacuum pump


34


. Refrigeration unit


26


also provides cooling to bring the chamber


22


to desired subfreezing temperatures. The pressure and temperature units


24


and


34


provide for creating atmospheric conditions which facilitate sublimation within the processing chamber


22


.




Referring now to

FIG. 2

, the microwave lyophilization system


20


also includes a microwave generation system. One or more magnetrons


40


are in connection with a power unit


32


to generate microwaves directed into the chamber


22


. In a preferred embodiment, wave guides


42


lead from each magnetron


40


to the processing chamber


22


. To optimize delivery of microwaves and coverage of materials in the chamber


22


, wave guides


42


may twist and bend with directional couplings


88


to direct microwaves into the chamber


22


at a desired location and orientation. Although the system is shown with each wave guide


42


having its own associated magnetron


40


, and vice versa, other configurations are possible with a single magnetron


40


or other numbers of magnetrons and wave guides


42


to generate substantially uniform microwave coverage within the processing chamber


22


. Each magnetron


40


could power more than one wave guide opening


80


.




Referring to

FIGS. 6

,


7


and


8


, as the chamber


22


is under vacuum with appropriate temperature and pressure ranges, a seal must be formed that can accommodate these pressures and maintain vacuum within the chamber


22


. Choke flanges


46


, wave guide window flanges


48


, and complementary flanges


47


are utilized within the wave guides


42


. The wave guide window flanges


48


lock a sealed wave guide window


44


within the wave guide


42


. The wave guide window


44


is typically made of a material such as TeflonĀ® that allows microwaves to pass through the window


44


. The wave guide window


44


has seals to maintain the chamber vacuum and pressures. It also separates the wave guide generators


40


from vacuum, so that modifications to accommodate the pressure ranges are not needed. As explained hereinafter, corona discharge and arcing is a common problem with microwave processing. Therefore, a temperature sensor


52


is placed in the wave guide window flange


48


mounting to the choke flange


46


. The wave guide window flange


48


may have a channel


50


formed therein for receiving the temperature sensor. With this configuration, temperature sensors


52


are shielded from the microwaves, yet are adjacent the wave guide window


44


where corona discharge may occur. Therefore, changes in temperature from an arc near the wave guide window


44


can be accurately detected with a sensor


52


extending downward in the choke flange


46


. As the sensor


52


does not insert directly into the path of the microwave field, and is therefore shielded from direct exposure to the microwaves, it presents no surface which might be conducive to corona discharge arc.




Referring to

FIG. 3

, the processing chamber


20


must also be configured with arc inhibiting surfaces so that corona discharge is minimized and preferably eliminated. Therefore, the chamber


22


is configured so that materials having surfaces that may lead to corona discharge, including metallic fasteners, such as bolts and rivets, are eliminated or the materials are shielded, so that corona discharge cannot arc to the surfaces. In addition, the chamber


22


includes sensors


82


that include shielding


84


or may be made from non-metallic fiber optic materials. The sensors


82


may be temperature sensors, optical sensors, such as photo detectors, or other sensors capable of corona discharge detection, and are typically positioned in a spaced apart relationship to form a sensor array. The interior of the processing chamber


22


may be made of materials such as polypropylene with shelf supports


62


molded or attached to the walls of the chamber


22


. Referring to

FIG. 9

, the chamber


22


may also include a shielded sensor cluster


86


having several sensors


82


grouped together and directed in various directions to cover the chamber


22


.




As shown in

FIGS. 3

,


5


and


9


, mode stirrers


70


may be located in the chamber


22


to redirect microwaves so that substantially the entire chamber


22


receives sufficiently uniform exposure to the microwaves. The mode stirrers


70


have a very slow rotation, but redirect microwaves sufficiently to expose the chamber


22


to achieve substantially complete microwave coverage. The stirrers


70


typically include blades


72


that include round shafts and preferably include rounded ends


74


for arc resistance. While the materials may be metallic, the surfaces are arc inhibiting, so that there are no sharp locations at which a discharge can be easily ignited. The welds and other attachments must be ground and smooth so that edges and points for arcing are not created. In addition to rounded elements, the shaft


76


of each stirrer


70


is shielded by a rounded bell-type housing


78


. The shielding


78


covers stirrer bearings and other potentially sharp edges that are utilized for rotation and for extension of the stirrer


70


into the lyophilizing chamber


22


.




The interior of the processing chamber


22


also includes openings


80


to the wave guides spaced about the chamber. As stated above, the chamber


22


may accommodate a number of different configurations of wave guides


42


that provide adequate coverage and exposure to the chamber


22


. Greater or lesser power may be utilized with various configurations to provide sufficient microwave strength to optimize the freeze drying process.




In addition to temperature and pressure considerations, the chamber


22


must also be configured to contain the microwaves therein. The opening leading to the condenser or vapor trap


24


must include a shielding screen


68


. The screen


68


must be configured to have sufficient openings for vapor flow, so that the air and/or water vapor entering the condenser has a sufficient flow rate to remove the water vapor from the processing chamber


22


and minimize the pressure differential between the chamber


22


and the condenser


24


. However, the screen


68


must be configured so that the openings are sized to prevent radiation having a wave length of microwaves from passing through the screen


68


and heating material in the condenser


24


. The door


92


, window


90


and the walls of the chamber


22


are also designed to minimize microwave exposure to objects outside the lyophilization system


20


.




Referring to

FIG. 6

, the sensors


52


in the window flanges


48


, and the sensors


82


in the chamber


22


, shown in

FIG. 3

, are in communication with a controller or central processing unit


38


. The controller


38


accepts input from the various sensors


82


within the chamber


22


and the other components and provides control to those components. For example, if the temperature sensors provide indications of increased temperature, the microwave power to the processing chamber


22


or to a portion of the chamber


22


is manually or automatically adjusted. Therefore, a spike in the temperature due to a corona discharge will be processed by the controller


38


to determine which sensors


82


and/or


52


are detecting a temperature increase and modifying the power output of an associated magnetron


40


or combination of magnetrons accordingly to eliminate corona discharge. The sensors


52


and


82


may also include other sensor types, such as photo detectors that detect a flash from each occurrence of corona discharge. The controller


38


may also take input from sensors


82


that provide feedback on pressure and temperature within the chamber. The controller


38


provides for monitoring as well as controlling the various processes and steps that occur during the lyophilization process. The controller


38


is also utilized to monitor the length of the power cycle and the various power levels depending on the requirements of the product undergoing processing. The controller


38


utilizes processing information from prior processed batches to provide optimal settings for various inputs and to optimize adjustments as processing occurs.




OPERATION




To begin the lyophilization process, the refrigeration unit


26


is activated and monitored, as shown in FIG.


4


. Following activation of the refrigeration unit


26


, the condenser


24


is also energized and its temperature controlled. The condenser


24


is cooled until predetermined temperature values have been obtained, and the vacuum pump


34


is activated and pressures monitored.




The present invention provides a system


20


that may be operated as a conventional lyophilizer using conduction, radiation and/or convection energy without microwaves, operated with a combination of conventional lyophilization and microwave energy, and operated using only microwave energy to facilitate lyophilization. When the chamber atmospheric conditions have reached a temperature and vacuum combination at which sublimation will occur, the magnetrons


40


are energized followed by the sensors including pressure and temperature sensors in the processing chamber


22


. The controller


38


utilizes stored information from previous processing to initialize power levels and other settings and make adjustments throughout the processing for optimizing processing. The microwave stirrers


70


are also energized so that the microwave field is dispersed in a pattern that substantially uniformly reaches all the product within the chamber


22


. The processing chamber


22


is continually monitored to determine whether incipient and/or actual corona discharges occur. If an incipient or actual corona discharge arc is detected, microwave power is reduced or shut off and the time and power level is recorded. Maximum settings may be adjusted accordingly. Chamber conditions may then be adjusted to proceed with processing without repeat of the corona discharge problems. Power may then be increased to the magnetrons


40


to a level which facilitates freeze drying, but does not create corona discharge as under previous conditions. In addition to adjusting the power of the magnetrons, and therefore the power of the microwaves in the processing chamber


22


, the vacuum and temperature may be adjusted to optimize the freeze drying operation.




When the temperature, vacuum and microwave power levels have all been set at optimal values for the most efficient lyophilization without causing corona discharge, the lyophilization process is continued. Throughout the process, the product temperature, microwave power and selection of magnetrons activated are monitored to make sure they do not exceed predetermined values so that the lyophilization operation may continue without compromising quality. As the lyophilization process continues, typically the microwaves will be adjusted utilizing on/off controls and/or variable power controls to ensure efficient sublimation of the ice. These controlled variations are optimized utilizing data from multiple collection points.




When the lyophilization process has been completed, as determined by reaching a predetermined moisture content and/or having reached a predetermined operating time, the process may be shut down. The product may be held at a predetermined temperature for a predetermined period under vacuum and sealed in its vials. Sealing is performed by compressing a stopper into the vial prior to or following repressurization with air or inert gas. In operations in which the product is held in trays, the product is simply unloaded. When the product has been unloaded, the refrigeration is turned off and the condenser


24


is defrosted and drained.




It is to be understood, however, that even though numerous characteristics and advantages of the present invention have been set forth in the foregoing description, together with details of the structure and function of the invention, the disclosure is illustrative only, and changes may be made in detail, especially in matters of shape, size and arrangement of parts within the principles of the invention to the fill extent indicated by the broad general meaning of the terms in which the appended claims are expressed.



Claims
  • 1. A lyophilizer system, adapted for operation in two modes, comprising:a lyophilizing chamber, including shielding from microwaves; a vacuum pumping system for creating vacuum in the lyophilizing chamber; a microwave generator, directing microwaves into the lyophilizing chamber; a refrigeration system for lowering the temperature of the lyophilizing chamber; chamber operating controls for creating a chamber environment in a first mode having a temperature and a pressure that is sufficient to facilitate sublimation in the chamber, and for creating a chamber environment in a second mode having sufficient vacuum and temperature such that when combined with microwaves directed into the chamber, facilitates sublimation in the chamber; a water vapor removal system located in or connected to the lyophilizing chamber for collecting water vapor from the lyophilizing chamber.
  • 2. A lyophilizer system according to claim 1, wherein the lyophilizing chamber further comprises shielding from microwaves.
  • 3. A lyophilizer system according to claim 1, further comprising a corona discharge detection system.
  • 4. A lyophilizer system according to claim 3, further comprising a corona discharge control system for controlling power of the microwave generator in response to the corona discharge detection system.
  • 5. A lyophilizer system according to claim 1, further comprising a microwave shielding screen intermediate the lyophilizing chamber and the condenser.
  • 6. A lyophilizer system according to claim 1, wherein the microwave generator includes a plurality of microwave generators selectively arranged to direct microwaves at all of the material to be lypohilized in the chamber.
  • 7. A lyophilizer system according to claim 1, further comprising a corona discharge detection and control system linked to the microwave generator for selectively varying power to the microwave generator.
  • 8. A lyophilizer system according to claim 6, further comprising a corona discharge detection and control system linked to the plurality of microwave generators for selectively varying power to each of the microwave generators.
  • 9. A microwave lyophilizer, comprising:a product processing chamber; a plurality of microwave generators and associated wave guides directed to the processing chamber, creating a microwave field; corona discharge detection system, having at least one sensor monitoring atmospheric conditions in the processing chamber; a controller connected to the sensors and selectively varying the power of the microwave generators in response to detected atmospheric changes in the processing chamber.
  • 10. A microwave lyophilizer according to claim 9, further comprising shielding for removing the sensors from direct exposure to the microwave field.
  • 11. A microwave lyophilizer according to claim 10, wherein the shielding comprises arc inhibiting surfaces in the processing chamber.
  • 12. A microwave lyophilizer according to claim 10, wherein the sensors comprise temperature sensors.
  • 13. A microwave lyophilizer according to claim 9, further comprising a refrigeration system and a pressurization system to create conditions that facilitate sublimation.
  • 14. A microwave lyophilizer according to claim 11, wherein the temperature sensors comprise non-arcing fiber optic materials.
  • 15. A microwave lyophilizer according to claim 12, wherein the temperature sensors are exterior of the microwave field.
  • 16. A microwave lyophilizer according to claim 10, wherein the sensors comprise photo detectors.
  • 17. A microwave lyophilizer according to claim 9, further comprising a microwave stirrer in the lyophilizing chamber.
  • 18. A microwave lyophilizer according to claim 17, wherein the stirrer includes shielding and arc inhibiting surfaces.
  • 19. A microwave system, comprising:a microwave chamber; microwave generators forming a microwave field in the chamber; a corona discharge detection system having at least one sensor monitoring the microwave chamber for occurrences of corona discharge; a generator controller in communication with the sensor and controlling power to the generators in response to detected discharges.
  • 20. A microwave system according to claim 19, wherein the sensor is shielded from microwaves.
  • 21. A microwave system according to claim 20, wherein the sensor comprises a temperature sensor.
  • 22. A microwave system according to claim 19, further comprising microwave stirrers within the microwave chamber.
  • 23. A microwave system according to claim 22, wherein the stirrers include arc inhibiting shielding.
  • 24. A microwave system according to claim 22, further comprising wave guides directing microwaves into the microwave chamber at predetermined orientations and spacing.
  • 25. A corona discharge control system for a microwave freeze dryer comprising:a microwave generator; at least one temperature sensor for sensing temperature increases in the freeze dryer; a comparator for comparing the measured temperature to a desired temperature range; controllers for controlling power of the microwave generator in response to signals from the comparator indicating detected variances from the desired temperature range, reflected power and/or light level.
  • 26. A corona discharge control system according to claim 25, further comprising arc inhibiting shielding on the sensor.
  • 27. A corona discharge control system according to claim 25, wherein the system includes a plurality of the sensors distributed in a spaced apart pattern forming a sensor array.
  • 28. A lyophilizer system, adapted for operation in two modes, comprising:a lyophilizing chamber; a vacuum pump for creating vacuum in the lyophilizing chamber; a microwave generator, directing microwaves into the lyophilizing chamber; a refrigeration system for lowering the temperature of the lyophilizing chamber; chamber operating controls for creating a chamber environment in a first mode using solely microwaves to facilitate sublimation in the chamber, and for creating a chamber environment in a second mode having sufficient vacuum and temperature such that when combined with microwaves directed into the chamber, facilitates sublimation in the chamber; a water vapor removal system located in or connected to the lyophilizing chamber for collecting water vapor from the lyophilizing chamber.
  • 29. A lyophilizer system, adapted for operation in two modes, comprising:a lyophilizing chamber; a vacuum pump for creating vacuum in the lyophilizing chamber; a microwave generator, directing microwaves into the lyophilizing chamber; a refrigeration system for lowering the temperature of the lyophilizing chamber; chamber operating controls for creating a chamber environment in a first mode having a temperature and a pressure that is sufficient to facilitate sublimation in the chamber, and for creating a chamber environment in a second mode using solely microwaves to facilitate sublimation in the chamber; a water vapor removal system located in or connected to the lyophilizing chamber for collecting water vapor from the lyophilizing chamber.
  • 30. A lyophilizer system, adapted for operation in three modes, comprising:a lyophilizing chamber; a pressure controller for creating vacuum in the lyophilizing chamber; a microwave generator, directing microwaves into the lyophilizing chamber; a refrigeration system for lowering the temperature of the lyophilizing chamber; chamber operating controls for creating a chamber environment in a first mode having a temperature and a pressure that is sufficient to facilitate sublimation in the chamber, for creating a chamber environment in a second mode having sufficient vacuum and temperature such that when combined with microwaves directed into the chamber, facilitates sublimation in the chamber, and for creating a chamber environment in a third mode using solely microwaves to facilitate sublimation in the chamber; and a water vapor removal system located in or connected to the lyophilizing chamber for collecting water vapor from the lyophilizing chamber.
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Corona Discharge Detection and Measurement, Intertec Publishing Corp. http://www.pcim.com/articles/1998/art0004/art1.html