CN100346190C - Microscope observation system during freezing dry process - Google Patents
Microscope observation system during freezing dry process Download PDFInfo
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- CN100346190C CN100346190C CNB200610049772XA CN200610049772A CN100346190C CN 100346190 C CN100346190 C CN 100346190C CN B200610049772X A CNB200610049772X A CN B200610049772XA CN 200610049772 A CN200610049772 A CN 200610049772A CN 100346190 C CN100346190 C CN 100346190C
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Abstract
The present invention discloses a microscope observation system during a freezing dry process, which is composed of an inverted type optical microscope with an automatic objective table, a freeze drying table, a cold quantity supplier, a vacuum device, a computer data acquisition control system, etc., wherein a digital video camera is arranged on the inverted type optical microscope, and the motion of the objective table is controlled by a computer. The freeze drying table is arranged on the objective table, the frozen sample is arranged on the freeze drying table, and the cooling / heating rate of the sample and the temperature gradient are all adjustable. In the long time drying process, a position of a sublimation interface can be obtained by a method of on-line processing micro pictures by the computer, and thus, the movement of the objective table is controlled, and the sublimation interface can be ensured to be always positioned in the microscopic field. The liquid nitrogen is consumed in a process of refrigeration by the present invention, and the liquid nitrogen does not consumed in a drying process. Because the freezing time is relatively short in the freeze-drying process, the drying time is relatively long, the present invention has the advantages of liquid nitrogen economization and reduction of test cost.
Description
Technical field
The present invention relates to a kind of system that is used for the freezing dry process microexamination.
Background technology
Freeze drying is called for short freeze-drying, and promptly elder generation by the freezing ice that becomes, will ice the water in the material distillation by vacuum and heating again, thereby remove the moisture in the material.Freeze-drying has important application in pharmacy, biomaterial preservation and food processing field.Many medicines adopt the freeze-drying mode to make pulvis, compare with the liquid injection, and pulvis can steady in a long-termly be preserved, convenient transportation.Compare with traditional cryopreservation biomaterial means, the storage of the biomaterial that the process freeze-drying is handled does not need low temperature, thereby saves a large amount of storages and trucking costs.Food adopts freeze-drying to handle the form in the time of not only can keeping fresh, and nutritional labeling and physiologically active ingredient retention rate height.Compare with frozen food, the storage fee of frozen dried food is with much lower.Freeze-drying is a complex physicochemical process, has a lot of phenomenons to be worth research, as the relation of carrying out speed and various factors of primary drying process.
Summary of the invention
The purpose of this invention is to provide a kind of system that is used for the freezing dry process microexamination.
It comprises inversion type optical microscope, freeze-drying platform, cold feedway, vacuum plant and the computer data acquiring control system of being with automatic carrier, the freeze-drying platform has the copper pedestal, on the copper pedestal, be provided with first thermoelectric element and second thermoelectric element, at the two thermoelectric elements microslide of having put on the shelf, at the copper pedestal vacuum (-tight) housing of having put on the shelf; The cold feedway has liquid nitrogen container, is provided with heat interchanger, well heater in liquid nitrogen container, and the escape pipe of liquid nitrogen container and first solenoid valve, freeze-drying platform, second solenoid valve join; Vacuum plant has vacuum pump, vacuum controller; The computer data acquiring control system has computing machine, and computing machine joins with silicon controlled module, relay module, logging, controllable direct current power supply, objective table drive unit respectively; Silicon controlled module output is joined with well heater, and relay module output is joined with vacuum pump, and controllable direct current power supply output is joined with first thermoelectric element and second thermoelectric element respectively.
Described copper pedestal top periphery has the sealed groove of placing vacuum (-tight) housing.The copper pedestal is a hollow rectangular parallelepiped, and copper base bottom central authorities have through hole, and the copper base bottom vertically has through hole, and copper pedestal upper lateral has through hole.Has a rectangle pit in the middle of the microslide.
The present invention only consumes liquid nitrogen in refrigerating process, then do not consume liquid nitrogen in dry run.Because the cooling time of freezing dry process is shorter relatively, and drying time is long.Thereby significant advantage of the present invention is to save liquid nitrogen, minimizing experimental cost.
Description of drawings
Fig. 1 is the system architecture synoptic diagram that is used for the freezing dry process microexamination;
Fig. 2 (a) is a copper pedestal three-dimensional view of the present invention;
Fig. 2 (b) is a copper pedestal sectional view of the present invention;
Among the figure: liquid nitrogen container 1; heat interchanger 2; well heater 3; vacuum pump 4; vacuum controller 5; solenoid valve 6; objective table 7; gas-distributing pipe 8; vacuum (-tight) housing 9; microslide 10; cover glass 11; transparent glass 12; object lens 13; sample 14; copper pedestal 15; objective table drive unit 16; solenoid valve 17; discharge 18; protective cover 19; transparent glass 20; condenser 21; thermopair 22; thermoelectric element 23; thermoelectric element 24; vacuum adapter 25; stop valve 26; nitrogen cylinder 27; protective cover 28; microscope pedestal 29; camera 30; silicon controlled module 31; relay module 32; computing machine 33; logging 34; controllable direct current power supply 35.
Embodiment
As shown in Figure 1, the system that is used for the freezing dry process microexamination comprises inversion type optical microscope, freeze-drying platform, cold feedway, vacuum plant and the computer data acquiring control system of being with automatic carrier, the freeze-drying platform has copper pedestal 15, on the copper pedestal, be provided with first thermoelectric element 23 and second thermoelectric element 24, at the two thermoelectric elements microslide 10 of having put on the shelf, at the copper pedestal vacuum (-tight) housing 9 of having put on the shelf; The cold feedway has liquid nitrogen container 1, is provided with heat interchanger 2, well heater 3 in liquid nitrogen container, and the escape pipe of liquid nitrogen container and first solenoid valve 6, freeze-drying platform, second solenoid valve 17 join; Vacuum plant has vacuum pump 4, vacuum controller 5; The computer data acquiring control system has computing machine 33, and computing machine joins with silicon controlled module 31, relay module 32, logging 34, controllable direct current power supply 35, objective table drive unit 16 respectively; Silicon controlled module 31 outputs are joined with well heater 3, and relay module 32 outputs are joined with vacuum pump 4, and controllable direct current power supply 35 outputs are joined with first thermoelectric element 23 and second thermoelectric element 24 respectively.
As shown in Figure 2, copper pedestal 15 top periphery of the present invention have the sealed groove of placing vacuum (-tight) housing 9.Copper pedestal 15 is hollow rectangular parallelepipeds, and copper base bottom central authorities have through hole, and the copper base bottom vertically has through hole, and copper pedestal upper lateral has through hole.
The present invention is used for the system of freezing dry process microexamination, is made up of five parts such as inversion type optical microscope, freeze-drying platform, cold feedway, vacuum plant and computer data acquiring control system of band automatic carrier.Digital stylus is installed on the inversion type optical microscope, can takes the image under the microscopic field, image enters computing machine by image collection card.Microscopical objective table is automatically, promptly is subjected to the control of computing machine, and computing machine is accurately located objective table by built-in step motor drive card, objective table drive unit.
The freeze-drying platform is placed on the microscopical objective table, and observed sample then is placed on the microslide.The freeze-drying platform is made up of the good copper pedestal of thermal conductivity, two thermoelectric elements, vacuum (-tight) housing, microslides, passes through for guaranteeing light, is embedded with glass sheet on vacuum (-tight) housing, for guaranteeing sealing, is wiped with vacuum grease at vacuum (-tight) housing and copper pedestal contact position.The structure of microslide is comparatively special, and the groove of a rectangle is left in the centre, and observed sample just is placed in this groove.After covered, the outlet of water vapor just has only one in the dry run, is convenient to like this dry run is carried out quantitative examination.Thermoelectric element is a two-stage, and its effect has two aspects, and the first provides cold in dry run, and the temperature of sample is remained on below the eutectic point, saves liquid nitrogen, and it two is that the thermograde of striding sample is provided in the sample refrigerating process.The latter's implementation method is to allow two thermoelectric elements be operated under the different states, and the adjustment of duty is finished by computing machine, controllable direct current power supply, and the temperature that thermopair records is the foundation of regulating.The thermograde of striding sample will influence the formation and the growth of ice crystal, and the shape and size of ice crystal will directly influence the carrying out of dry run.Be arranged in the copper pedestal central authorities punching under the thermoelectric element, be inlaid with glass sheet in the hole, purpose is to allow light pass through, and also leaves the duct that cold nitrogen passes through in the copper pedestal.In the refrigerating process of sample, the pipeline of cold is: cold nitrogen → copper pedestal → thermoelectric element → microslide → sample.On the freeze-drying platform, also have protective cover, logical drying nitrogen in the cover, purpose is the generation that prevents dewfall or frosting phenomenon.
The cold feedway comprises liquid nitrogen bottle, is arranged in heat interchanger, well heater and two solenoid valves in the liquid nitrogen bottle.What of cold nitrogen flow are the size that adds heat determine, determined by computing machine, realize by the silicon controlled module control heater.Become nitrogen after liquid nitrogen is heated, nitrogen is transported to the freeze-drying platform after heat interchanger is cooled near liquid nitrogen temperature.The solenoid valve of on cold nitrogen pipeline, arranging, after refrigerating process finishes, closed electromagnetic valve, well heater is also out of service simultaneously.
Vacuum plant comprises vacuum pump, vacuum controller.The effect of vacuum controller be guarantee sample space be in certain vacuum tightness (as ~ 8Pa) under.Whether vacuum pump starts and is subjected to computer control, realizes by relay module.Be to guarantee the vacuum of sample space, the thermocouple wire of drawing from the freeze-drying platform, thermoelectric element wiring are all by being contained in the vacuum adapter in the copper pedestal.
The computer data acquiring control system comprises computing machine and various interface module.Data acquisition control card, stepping motor control card, image collection card are housed in the computing machine.Data acquisition to as if thermocouple signal, its is converted into digital signal through logging, enters computing machine by serial line interface.The object that computing machine will be controlled comprises objective table drive unit, thermoelectric element, well heater, solenoid valve, vacuum pump, wherein solenoid valve, vacuum pump control need digital signal, the objective table driving device controls needs digital pulse signal, and thermoelectric element and well heater control need simulating signal.Stepping motor control card output digital pulse signal, data acquisition control card output digital signal and simulating signal are controlled the operation of each object respectively.Image collection card is responsible for the collection of microscopic image, and the picture information after the collection with the document form storage, is handled for image processing program on the one hand on the other hand in real time.
The step that the present invention carries out the freezing dry process microexamination is as follows: 1) sample is placed in the groove of microslide covered; 2) build vacuum (-tight) housing and protective cover, adjust condenser and objective lens, obtain the sharp image of sample; 3) in protective cover, feed drying nitrogen; 4) open liquid nitrogen bottle interior well heater and solenoid valve, start temperature-fall period, that regulates well heater adds heat to regulate the flow of cold nitrogen, and sample is cooled to below the eutectic temperature with given pace; 5) start electrothermal module, make it be operated in refrigeration mode, close well heater and solenoid valve then, keep sample temperature constant substantially; 6) start vacuum pump, make sample space vacuum tightness reach setting value fast; When 7) distillation of the ice in sample is for water vapor, the distillation interface can slowly be moved, time can continue a few hours, during this period, computing machine is according to the image analysis distillation position, interface that collects, when field of view was shifted out soon in the distillation interface, the computer control automatic carrier was mobile slightly, was in the field of view all the time to guarantee the distillation interface; When 8) ice in sample was sublimate into prior desired location, experiment stopped.
Claims (4)
1 one kinds of systems that are used for the freezing dry process microexamination, it is characterized in that, it comprises inversion type optical microscope, freeze-drying platform, cold feedway, vacuum plant and the computer data acquiring control system of being with automatic carrier, the freeze-drying platform has copper pedestal (15), on the copper pedestal, be provided with first thermoelectric element (23) and second thermoelectric element (24), at the two thermoelectric elements microslide (10) of having put on the shelf, at the copper pedestal vacuum (-tight) housing (9) of having put on the shelf; The cold feedway has liquid nitrogen container (1), is provided with heat interchanger (2), well heater (3) in liquid nitrogen container, and the escape pipe of liquid nitrogen container and first solenoid valve (6), freeze-drying platform, second solenoid valve (17) join; Vacuum plant has vacuum pump (4), vacuum controller (5); The computer data acquiring control system has computing machine (33), and computing machine joins with silicon controlled module (31), relay module (32), logging (34), controllable direct current power supply (35), objective table drive unit (16) respectively; Silicon controlled module (31) output is joined with well heater (3), and relay module (32) output is joined with vacuum pump (4), and controllable direct current power supply (35) output is joined with first thermoelectric element (23) and second thermoelectric element (24) respectively.
2. a kind of system that is used for the freezing dry process microexamination according to claim 1 is characterized in that, described copper pedestal (15) top periphery has the sealed groove of placing vacuum (-tight) housing (9).
3. a kind of system that is used for the freezing dry process microexamination according to claim 1, it is characterized in that described copper pedestal (15) is a hollow rectangular parallelepiped, copper base bottom central authorities have through hole, the copper base bottom vertically has through hole, and copper pedestal upper lateral has through hole.
4. a kind of system that is used for the freezing dry process microexamination according to claim 1 is characterized in that, has a rectangle pit in the middle of the described microslide (10).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610049772XA CN100346190C (en) | 2006-03-10 | 2006-03-10 | Microscope observation system during freezing dry process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610049772XA CN100346190C (en) | 2006-03-10 | 2006-03-10 | Microscope observation system during freezing dry process |
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| CN1818738A CN1818738A (en) | 2006-08-16 |
| CN100346190C true CN100346190C (en) | 2007-10-31 |
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| CNB200610049772XA Expired - Fee Related CN100346190C (en) | 2006-03-10 | 2006-03-10 | Microscope observation system during freezing dry process |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101793458B (en) * | 2010-04-02 | 2012-03-21 | 中山大学 | Vacuum freezing drying device with functions of DSC and microstructure observation |
| CN104634736A (en) * | 2013-11-15 | 2015-05-20 | 中国科学院生物物理研究所 | Three-dimensional automatic ultralow-temperature sample stage for iPALM (interferometric photoactivated localization microscopy) microscope |
| GB2551687A (en) * | 2016-03-04 | 2018-01-03 | Linkam Scient Instruments Ltd | Freeze drying apparatus |
| CN108873297A (en) * | 2018-09-15 | 2018-11-23 | 乔燕春 | A kind of object stage for microscope and the freeze-drying microscope being made of it |
| CN113655057A (en) * | 2021-08-24 | 2021-11-16 | 威世药业（如皋）有限公司 | Equipment for detecting influence of freeze drying treatment on vaccinia virus virulence |
| CN114967097A (en) * | 2022-06-29 | 2022-08-30 | 东富龙科技集团股份有限公司 | Temperature control system of freeze-drying microscope objective table |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2337487Y (en) * | 1998-03-25 | 1999-09-08 | 浙江大学 | Freeze-drying box for freeze dryer |
| JPH11264659A (en) * | 1998-03-09 | 1999-09-28 | Hal Co Division Of Sp Ind Inc | Method and device for freeze drying |
| JP2004232883A (en) * | 2003-01-28 | 2004-08-19 | Ulvac Japan Ltd | Spray type vacuum freeze-drying device |
| CN1208739C (en) * | 2003-04-16 | 2005-06-29 | 浙江大学 | Computer controlled low temperature biology microscopic system |
-
2006
- 2006-03-10 CN CNB200610049772XA patent/CN100346190C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11264659A (en) * | 1998-03-09 | 1999-09-28 | Hal Co Division Of Sp Ind Inc | Method and device for freeze drying |
| CN2337487Y (en) * | 1998-03-25 | 1999-09-08 | 浙江大学 | Freeze-drying box for freeze dryer |
| JP2004232883A (en) * | 2003-01-28 | 2004-08-19 | Ulvac Japan Ltd | Spray type vacuum freeze-drying device |
| CN1208739C (en) * | 2003-04-16 | 2005-06-29 | 浙江大学 | Computer controlled low temperature biology microscopic system |
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| CN1818738A (en) | 2006-08-16 |
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Assignee: Hangzhou Aoya Bio-Tech. Co., Ltd. Assignor: Zhejiang University Contract record no.: 2011330000643 Denomination of invention: Microscope observation system during freezing dry process Granted publication date: 20071031 License type: Exclusive License Open date: 20060816 Record date: 20110531 |
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Granted publication date: 20071031 Termination date: 20180310 |
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| CF01 | Termination of patent right due to non-payment of annual fee |