CN115032782A - Low-temperature freeze-drying objective table - Google Patents

Low-temperature freeze-drying objective table Download PDF

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Publication number
CN115032782A
CN115032782A CN202210748744.6A CN202210748744A CN115032782A CN 115032782 A CN115032782 A CN 115032782A CN 202210748744 A CN202210748744 A CN 202210748744A CN 115032782 A CN115032782 A CN 115032782A
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China
Prior art keywords
temperature
sample chamber
vacuum
connection port
objective table
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CN202210748744.6A
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Chinese (zh)
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马丹萍
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Tofflon Science and Technology Group Co Ltd
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Tofflon Science and Technology Group Co Ltd
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Priority to CN202210748744.6A priority Critical patent/CN115032782A/en
Publication of CN115032782A publication Critical patent/CN115032782A/en
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/34Microscope slides, e.g. mounting specimens on microscope slides
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/24Base structure
    • G02B21/28Base structure with cooling device
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/24Base structure
    • G02B21/30Base structure with heating device

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a low-temperature freeze-drying objective table, which comprises an objective table shell; a measurement sample chamber disposed within the stage housing; a temperature adjusting mechanism disposed in the measurement sample chamber; the pressure adjusting mechanism connected with the measuring sample chamber is arranged on the sample fixer mechanism in the measuring sample chamber; and a sample holder adjustment mechanism connected to a side of the stage housing; the object is to provide a low-temperature freeze-drying objective table aiming at the requirements of the existing biomedicine on a freeze-drying microscope objective table, which can work for a long time in a low-temperature and low-vacuum environment; the temperature control system has the advantages of uniform distribution of the temperature field in the sample chamber, high accuracy of temperature control and pressure control, high system stability and the like.

Description

Low-temperature freeze-drying objective table
Technical Field
The invention relates to a low-temperature freeze-drying objective table.
Background
The components and spatial structure of the biological products on the market are very complex, and the biological products are also very sensitive to temperature. In order to ensure the activity of the biological products, the biological products are protected by freezing and freeze-drying. In the two processes, the activity of the biological product is greatly influenced by the crystal forming and growing process when the biological product is crystallized. Therefore, we need to observe the change of crystallization during the freeze-drying process to explore the rule.
The low-temperature high-vacuum freeze-drying microscope can be used for observing various phenomena generated by a biological sample in a low-temperature high-vacuum environment, such as the formation of ice crystals inside and outside cells, the change of the external dimensions of the cells and the like. The freeze-drying microscope is used as a laboratory tool, can observe and research the structural change of a freeze-drying product in the freeze-drying process at a microscopic level, measures a key parameter of collapse temperature, provides data support for freeze-drying industrial production, guides the design and production of freeze-drying equipment, effectively shortens the period of groping freeze-drying curves, and improves the economic benefit of enterprises. A cryo-lyophilization stage is therefore proposed to address the above problems.
Disclosure of Invention
The invention aims to provide a low-temperature freeze-drying objective table aiming at the requirements of the existing biomedicine on a freeze-drying microscope objective table, which can work for a long time in a low-temperature low-vacuum environment; the temperature control system has the advantages of uniform distribution of the temperature field in the sample chamber, high accuracy of temperature control and pressure control, high system stability and the like.
The technical scheme for realizing the purpose is as follows: a low temperature freeze-drying stage comprises
An object stage housing;
a measurement sample chamber disposed within the stage housing;
a temperature adjusting mechanism disposed in the measurement sample chamber;
a pressure regulating mechanism connected with the measuring sample chamber;
a sample holder mechanism disposed within the measurement sample chamber; and
the sample fixer adjusting mechanism is connected to the side edge of the object stage shell;
wherein the upper port of the object stage shell is connected with a sealing cover; a bottom plate of the measurement sample chamber is provided with a light through hole, and the light through hole is conical.
Preferably, the temperature adjusting mechanism comprises a temperature module, the temperature module is connected with a heating element wire, and the heating element wire is connected with a lead interface arranged on the outer side wall of the object stage shell; the outer side wall of the objective table shell is also connected with two liquid nitrogen cooling interfaces, the two liquid nitrogen cooling interfaces are respectively connected with two high-thermal-conductivity metal pipes, and the two high-thermal-conductivity metal pipes are connected after being wound for one circle outside the temperature module; and the temperature module is also connected with a platinum resistor.
Preferably, the pressure adjusting mechanism includes a first vacuum connection port and a second vacuum connection port, the first vacuum connection port and the second vacuum connection port are respectively connected to two sides of the stage housing, and the first vacuum connection port and the second vacuum connection port are respectively communicated with the measurement sample chamber.
Preferably, the sample fixer mechanism comprises a rectangular block, the rear end of the rectangular block is connected with the hollow circular ring, and sliding grooves are formed in two sides of the rectangular block; the rectangular block is placed on the temperature module.
Preferably, the sample fixer adjusting mechanism comprises a fixed door bolt connected to the stage housing, the side edge of the fixed door bolt and the side wall of the stage housing are respectively connected to a y-axis adjusting knob and an x-axis adjusting knob, and the inner ends of the y-axis adjusting knob and the x-axis adjusting knob are connected to the sliding grooves formed in two sides of the rectangular block.
Preferably, the first vacuum connecting port and the second vacuum connecting port are both standard flange interfaces, and the first vacuum connecting port is connected with a vacuum pump; and the second vacuum connecting port is connected with a Pirani vacuum gauge.
Preferably, one surface of the sealing cover, which is in contact with the object stage shell, is provided with a rubber ring.
Preferably, the sealing cover is made of quartz glass material.
The invention has the beneficial effects that:
1. the rapid and accurate micro-freezing vacuum environment can be provided for biological engineering research personnel, the change process of crystals in the whole freeze-drying process can be observed, and the temperature and pressure data in the product freezing vacuum process can be measured. Can accurately measure the collapse temperature of the sample, the permeability of the biological material, the structural change of the cell freeze-drying process and the like.
2. The experimental data precision of temperature measurement and pressure measurement is high, and real-time pressure measurement and temperature measurement can be achieved.
3. The freezing, heating rates and system temperature ranges have a wide range of adjustments and still provide a continuous clear view after changes in stage chamber temperature.
4. The objective table has good tightness during operation, and the objective table and components thereof are not easy to damage under the pressure of about 1 atmosphere under the larger internal and external pressure difference.
5. The manufacturing process is simple, the materials are easy to obtain, and the device is suitable for long-term use and convenient to maintain.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a sample holder mechanism of the present invention;
figure 3 is a detailed view of the seal cap of the present invention.
In the figure: 1. a lead interface; 2. a liquid nitrogen cooling interface; 3. an object stage housing; 4. a heating element wire; 5. a high thermal conductivity metal tube; 6. a platinum resistor; 7. a temperature module; 8. a first vacuum connection port; 9. a second vacuum connection port; 10. measuring the sample chamber; 11. fixing the door bolt; 12. an x-axis adjustment knob; 13. a y-axis adjustment knob; 14. a rectangular block; 15. a hollow circular ring; 16. and (7) sealing the cover.
Detailed Description
The technical scheme of the invention is clearly and completely described in the following with reference to the accompanying drawings. In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance.
The invention will be further explained with reference to the drawings.
As shown in fig. 1-3, a cryo-lyophilization stage includes a stage housing 3; a measurement sample chamber 10 disposed in the stage housing 3; a temperature adjusting mechanism disposed in the measurement sample chamber 10; a pressure regulating mechanism connected with the measurement sample chamber 10; a sample holder mechanism disposed within the measurement sample chamber 10; and a sample holder adjusting mechanism connected to the side of the stage housing 3; wherein, the upper port of the objective table shell 3 is connected with a sealing cover 16; the bottom plate of the measurement sample chamber 10 is provided with a light through hole. The sealing cover 16 is provided with a rubber ring on the surface contacting with the stage housing 3. The sealing cover 16 is made of quartz glass material, and the light through hole is conical.
Specifically, the temperature adjusting mechanism comprises a temperature module 7, the temperature module 7 is connected with a heating element wire 4, the heating element wire 4 is connected with a lead interface 1 arranged on the outer side wall of the objective table shell 3, the heating power of the electric heating plate can be changed by changing the current, and the heating rate is further changed; the outer side wall of the objective table shell 3 is also connected with two liquid nitrogen cooling interfaces 2, the two liquid nitrogen cooling interfaces 2 are respectively connected with two high-thermal-conductivity metal tubes 5, the two high-thermal-conductivity metal tubes 5 are wound for a circle outside the temperature module 7 and then connected, and the cooling rate of the high-thermal-conductivity metal tubes 5 can be changed by changing the flow of liquid nitrogen in the high-thermal-conductivity metal tubes 5; the temperature module 7 is also connected with a platinum resistor 6, and the temperature of the upper surface of the temperature module 7 can be measured through the platinum resistor 6, so that the purpose of temperature measurement can be achieved.
Specifically, the pressure adjusting mechanism comprises a first vacuum connecting port 8 and a second vacuum connecting port 9, the first vacuum connecting port 8 and the second vacuum connecting port 9 are respectively connected to two sides of the stage housing 3, and the first vacuum connecting port 8 and the second vacuum connecting port 9 are respectively communicated with a measurement sample chamber 10. The first vacuum connecting port 8 and the second vacuum connecting port 9 are both standard flange interfaces, and the first vacuum connecting port 8 is connected with a vacuum pump; the second vacuum connecting port 9 is connected with a pirani vacuum gauge, and the vacuum-pumping treatment is carried out on the measurement sample chamber 10 through a vacuum pump, so that the pressure in the measurement sample chamber 10 can reach a low vacuum state; the pirani vacuum gauge is used for measuring the vacuum degree in the sample chamber 10, and when the vacuum degree required by the experiment is reached, the vacuum pump or the corresponding pressure valve can be adjusted to control the pressure.
Specifically, the sample fixer mechanism comprises a rectangular block 14, the rear end of the rectangular block 14 is connected with a hollow circular ring 15, and sliding grooves are formed in two sides of the rectangular block 14; the rectangular block 14 is placed on the temperature module 7. The hollow ring 15 is a region for placing a sample, and when performing an experiment, a glass slide is placed on the hollow ring 15, then the experimental sample is added, a cover glass is placed to cover the experimental sample, and then a freeze-drying experiment is performed.
Specifically, sample fixer adjustment mechanism includes fixed keeper 11, and fixed keeper 11 is connected on objective table shell 3, and y axle adjust knob 13 and x axle adjust knob 12 are connected respectively to fixed keeper 11 side and objective table shell 3 lateral wall, and the spout that the rectangle piece 14 both sides were seted up is connected to the inner of y axle adjust knob 13 and x axle adjust knob 12. The fixing bolt 11 is used for replacing the sample holder, the fixing bolt 11 is opened by unscrewing the fixing bolt 11, and then the sample holder is replaced, and the x-axis adjusting knob 12 and the y-axis adjusting knob 13 can adjust the position of the sample holder on the temperature module 7, so that the sample is positioned at the center of the temperature module 7.
The working principle is as follows: the temperature module 7 is connected with the heating element wire 4, the heating element wire 4 is connected with the lead interface 1 arranged on the outer side wall of the objective table shell 3, the heating power of the electric heating plate can be changed by changing the current, and the heating rate is further changed; the outer side wall of the objective table shell 3 is also connected with two liquid nitrogen cooling interfaces 2, the two liquid nitrogen cooling interfaces 2 are respectively connected with two high-thermal-conductivity metal tubes 5, the two high-thermal-conductivity metal tubes 5 are wound for a circle outside the temperature module 7 and then connected, and the cooling rate of the high-thermal-conductivity metal tubes 5 can be changed by changing the flow of liquid nitrogen in the high-thermal-conductivity metal tubes 5; the temperature module 7 is also connected with a platinum resistor 6, and the temperature of the upper surface of the temperature module 7 can be measured through the platinum resistor 6, so that the purpose of temperature measurement can be achieved. The first vacuum connecting port 8 is connected with a vacuum pump; the second vacuum connecting port 9 is connected with a pirani vacuum gauge, and the vacuum-pumping treatment is carried out on the measurement sample chamber 10 through a vacuum pump, so that the pressure in the measurement sample chamber 10 can reach a low vacuum state; the pirani vacuum gauge is used for measuring the vacuum degree in the sample chamber 10, and when the vacuum degree required by the experiment is reached, the vacuum pump or the corresponding pressure valve can be adjusted to control the pressure. The rear end of the rectangular block 14 is connected with a hollow circular ring 15, and sliding grooves are formed in two sides of the rectangular block 14; the rectangular block 14 is placed on the temperature module 7. The hollow ring 15 is a region for placing a sample, and when performing an experiment, a glass slide is placed on the hollow ring 15, then the experimental sample is added, a cover glass is placed to cover the experimental sample, and then a freeze-drying experiment is performed. Fixed keeper 11 is connected on objective table shell 3, and y axle adjust knob 13 and x axle adjust knob 12 are connected respectively to fixed keeper 11 side and objective table shell 3 lateral wall, and the spout that rectangle piece 14 both sides were seted up is connected to the inner of y axle adjust knob 13 and x axle adjust knob 12. The fixing bolt 11 is used to replace the sample holder mechanism, the fixing bolt 11 is opened by unscrewing the fixing bolt 11, and then the sample holder mechanism is replaced, and the x-axis adjusting knob 12 and the y-axis adjusting knob 13 are used to adjust the position of the sample holder mechanism on the temperature module 7, so that the sample is located at the center of the temperature module 7.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A low-temperature freeze-drying objective table is characterized by comprising
A stage housing (3);
a measurement sample chamber (10) arranged in the object stage housing (3);
a temperature regulating mechanism disposed within the measurement sample chamber (10);
a pressure regulating mechanism connected to the measurement sample chamber (10);
a sample holder mechanism disposed within the measurement sample chamber (10); and
the sample fixer adjusting mechanism is connected to the side edge of the objective table shell (3);
wherein the upper port of the object stage shell (3) is connected with a sealing cover (16); the bottom plate of the measurement sample chamber (10) is provided with a light through hole, and the light through hole is conical.
2. A cryolyophilization stage according to claim 1, wherein the temperature adjustment mechanism comprises a temperature module (7), the temperature module (7) is connected to a heating element wire (4), the heating element wire (4) is connected to a lead interface (1) arranged on an outer side wall of the stage housing (3); the outer side wall of the objective table shell (3) is also connected with two liquid nitrogen cooling interfaces (2), the two liquid nitrogen cooling interfaces (2) are respectively connected with two high-thermal-conductivity metal pipes (5), and the two high-thermal-conductivity metal pipes (5) are wound on the outer side of the temperature module (7) for a circle and then connected; and the temperature module (7) is also connected with a platinum resistor (6).
3. The cryogenic freeze-drying stage according to claim 2, wherein the pressure adjustment mechanism comprises a first vacuum connection port (8) and a second vacuum connection port (9), the first vacuum connection port (8) and the second vacuum connection port (9) are respectively connected to two sides of the stage housing (3), and the first vacuum connection port (8) and the second vacuum connection port (9) are respectively communicated with the measurement sample chamber (10).
4. The cryo-lyophilization stage according to claim 3, wherein the sample holder mechanism comprises a rectangular block (14), the rear end of the rectangular block (14) is connected with a hollow ring (15), and sliding grooves are formed on both sides of the rectangular block (14); the rectangular block (14) is placed on the temperature module (7).
5. The cryo-lyophilization stage according to claim 4, wherein the sample holder adjusting mechanism comprises a fixed bolt (11), the fixed bolt (11) is connected to the stage housing (3), the side of the fixed bolt (11) and the side wall of the stage housing (3) are respectively connected to a y-axis adjusting knob (13) and an x-axis adjusting knob (12), and the inner ends of the y-axis adjusting knob (13) and the x-axis adjusting knob (12) are connected to the sliding grooves formed on two sides of the rectangular block (14).
6. A cryogenic freeze drying stage according to claim 3, wherein the first vacuum connection port (8) and the second vacuum connection port (9) are both standard flange interfaces, the first vacuum connection port (8) being connected to a vacuum pump; the second vacuum connecting port (9) is connected with a Pirani vacuum gauge.
7. A lyophilization stage according to claim 1, wherein the side of the sealing cover (16) in contact with the stage housing (3) is provided with a rubber ring.
8. A lyophilization stage as claimed in claim 7, wherein the sealing cover (16) is of quartz glass material.
CN202210748744.6A 2022-06-29 2022-06-29 Low-temperature freeze-drying objective table Pending CN115032782A (en)

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Application Number Priority Date Filing Date Title
CN202210748744.6A CN115032782A (en) 2022-06-29 2022-06-29 Low-temperature freeze-drying objective table

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Application Number Priority Date Filing Date Title
CN202210748744.6A CN115032782A (en) 2022-06-29 2022-06-29 Low-temperature freeze-drying objective table

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN205427299U (en) * 2016-03-11 2016-08-03 宁波键一生物科技有限公司 Automatic regulating apparatus of objective table
CN108646038A (en) * 2018-04-17 2018-10-12 中国地质大学(武汉) A kind of temperature-control pressure-control sample stage and temperature and pressure control system
CN109246860A (en) * 2018-09-28 2019-01-18 暨南大学 In situ, dynamic observation material high temperature service under the microscope can be achieved
CN209055744U (en) * 2018-09-15 2019-07-02 乔燕春 A kind of object stage for microscope and the freeze-drying microscope being made of it
CN213023758U (en) * 2020-09-25 2021-04-20 兰州文理学院 Driving mechanism of microscope objective table
CN113721357A (en) * 2021-09-28 2021-11-30 上海理工大学 Device and system for ultrasonic ice-planting microscopic observation
CN113848636A (en) * 2021-11-10 2021-12-28 山东省科学院新材料研究所 Microscope object placing table and microscope comprising same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN205427299U (en) * 2016-03-11 2016-08-03 宁波键一生物科技有限公司 Automatic regulating apparatus of objective table
CN108646038A (en) * 2018-04-17 2018-10-12 中国地质大学(武汉) A kind of temperature-control pressure-control sample stage and temperature and pressure control system
CN209055744U (en) * 2018-09-15 2019-07-02 乔燕春 A kind of object stage for microscope and the freeze-drying microscope being made of it
CN109246860A (en) * 2018-09-28 2019-01-18 暨南大学 In situ, dynamic observation material high temperature service under the microscope can be achieved
CN213023758U (en) * 2020-09-25 2021-04-20 兰州文理学院 Driving mechanism of microscope objective table
CN113721357A (en) * 2021-09-28 2021-11-30 上海理工大学 Device and system for ultrasonic ice-planting microscopic observation
CN113848636A (en) * 2021-11-10 2021-12-28 山东省科学院新材料研究所 Microscope object placing table and microscope comprising same

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