A temperature-controllable vacuum stage

Abstract

This invention relates to a temperature-controllable vacuum stage, belonging to the field of freeze-drying technology. The stage comprises a stage shell, a fixing device located beneath the stage shell, a stage cap mounted on the stage shell, a top end cap at the top of the stage shell, a bottom end cap at the bottom of the stage shell, a sample platform located inside the stage shell, an X / Y axis displacement adjuster connected to the stage shell, and two vacuum connection ports connected to both sides of the stage shell. By using a temperature probe installed inside the sample platform to feedback and control the liquid nitrogen flow rate and electric heating power within the sample platform, the heating, cooling, and constant temperature control of the sample platform surface can be achieved. Furthermore, the collapse of the product can be observed in a vacuum environment, and the collapse temperature can be read, thereby shortening the development cycle of the freeze-drying process or optimizing existing freeze-drying processes.

Description

Technical Field

[0001] This invention belongs to the field of freeze-drying technology, and in particular relates to a vacuum stage with controllable temperature. Background Technology

[0002] Freeze-drying is frequently used in biological research and drug development to dry samples. Freeze-drying typically involves three processes: pre-freezing, primary drying, and secondary drying. The collapse temperature is a key parameter in the primary drying process. After pre-freezing, the product is heated during the drying stage. As the temperature gradually rises to a critical value, its rigid structure becomes insufficient to maintain its original three-dimensional structure, causing the product to collapse. This critical temperature is called the collapse temperature. During the primary drying stage, the temperature of the product must be controlled below its collapse temperature.

[0003] The collapse of the product is caused by changes in the microstructure during the freeze-drying process. The collapse initially occurs between the dried layer and the frozen layer of the product. The process of the product being slowly heated until it collapses under the freeze-drying vacuum conditions can be observed using a microscope, thereby determining the collapse temperature of the product, shortening the product development cycle, and optimizing the product freeze-drying process.

[0004] Most existing low-temperature stages can only provide observation environments at room temperature and pressure or only at low temperatures, and cannot provide a vacuum observation environment with precise temperature control. Moreover, most low-temperature stages have complex structures and, while lacking heating and constant temperature control, also have unresolved problems such as difficulty in aligning the light transmission aperture, poor sealing, difficulty in loading, and inability to adjust the observation area. Summary of the Invention

[0005] The purpose of this invention is to provide a stage that can provide a vacuum environment and precisely control the cooling, heating, and constant temperature of samples.

[0006] To achieve the above objectives, the present invention provides a temperature-controllable vacuum stage, comprising a stage shell, a fixing device disposed under the stage shell, a stage cap disposed on the stage shell, a top end cap disposed at the top of the stage shell, a bottom end cap disposed at the bottom of the stage shell, a sample platform disposed inside the stage shell, an X / Y axis displacement adjuster connected to the stage shell, and two vacuum connection ports connected to both sides of the stage shell; the liquid nitrogen flow rate and electric heating power within the sample platform are controlled by a temperature probe installed inside the sample platform, thereby achieving temperature rise, fall, and constant temperature control of the sample platform surface.

[0007] Preferably, the sample platform includes a liquid nitrogen inlet / outlet pipeline and an upper platform. One end of the liquid nitrogen inlet / outlet pipeline is connected to the two openings on the outside of the upper platform and communicates with the liquid nitrogen flow channel inside the upper platform. The other end passes through the opening of the top end cap and connects to the external liquid nitrogen inlet / outlet pipeline.

[0008] Preferably, the sample platform is provided with a flow channel plug, and the liquid nitrogen flow channel is provided on the lower side of the upper platform, which can fit with the flow channel plug; the upper platform is provided with a temperature measuring port, an electric heating fixing port and a cable outlet.

[0009] Preferably, the sample platform further includes a lower cover, and the annular electric heating element is fixed by an interference fit between the upper platform and the lower cover; the centers of the light-transmitting holes of the upper platform and the lower cover are aligned.

[0010] Preferably, the vacuum connection ports are installed on both sides of the stage housing; one is connected to a vacuum pump to evacuate the stage and create a vacuum environment inside the stage cavity; the other is connected to a vacuum gauge to read the vacuum level inside the stage cavity.

[0011] Preferably, the stage housing is provided with a positioning device and a light-transmitting window below it, which can be mounted on a microscope. The sample observation area can be adjusted by the X / Y axis displacement adjuster, and the sample can be observed through the viewing window above the stage cap.

[0012] Preferably, the stage housing includes an upper plate and a lower plate. The stage housing is placed on the microscope stage. The fixing device located below the stage housing is adjusted to align the center of the microscope light source and the light window on the lower side of the stage housing.

[0013] Preferably, the lower plate has a semi-circular stage for positioning the sample platform, so that the light-transmitting hole of the sample platform is aligned with the center of the light-transmitting window of the lower plate; the stage cap can be screwed onto the upper plate, and the cap window is aligned with the center of the light-transmitting hole of the sample platform.

[0014] Preferably, the top end cap has a liquid nitrogen inlet / outlet and an aviation plug, and the electric heating power cord and temperature probe signal line in the sample platform can be connected to external equipment via the aviation plug.

[0015] Preferably, the X / Y axis displacement adjuster includes an X-axis adjusting rod, an X-axis adjusting slider, a Y-axis adjusting rod, a Y-axis adjusting slider, an X / Y axis sealing ring, a slide rail, and a displacement pressure ring. The observation area of ​​the microscope is adjusted by moving the sample within the displacement pressure ring through the handwheels on the X-axis adjusting rod and the Y-axis adjusting rod.

[0016] In summary, the present invention has the following beneficial technical effects:

[0017] This invention enables temperature control of products within a stage, including cooling, heating, and constant temperature. It also allows observation of product collapse under vacuum conditions and reading of the collapse temperature, thereby shortening the development cycle of freeze-drying processes or optimizing existing freeze-drying techniques. The stage features excellent sealing, rapid alignment of the light aperture, X / Y axis displacement adjustment for easy adjustment of the observation area, convenient installation and fixation, and easy sample loading. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of a temperature-controllable vacuum stage according to the present invention.

[0019] Figure 2 This is a top view of the stage with its cap screwed on in this invention;

[0020] Figure 3 This is a front view of a temperature-controllable vacuum stage according to the present invention.

[0021] Figure 4 This is a left view of a temperature-controllable vacuum stage according to the present invention.

[0022] Figure 5 This is a bottom view of a temperature-controllable vacuum stage according to the present invention.

[0023] Figure 6 This is a schematic diagram of the sample platform structure in this invention;

[0024] Figure 7 This is a top view of the sample platform in this invention;

[0025] Figure 8 This is a schematic diagram of the structure of the stage shell in this invention;

[0026] Figure 9 This is a bottom view of the stage housing in this invention;

[0027] Figure 10 This is a schematic diagram of the X / Y displacement adjustment device in this invention;

[0028] Figure 11 This is a schematic diagram of the X-axis adjusting rod structure in this invention.

[0029] Reference numerals: 1. Stage housing; 2. Fixing device; 3. Stage cap; 4. Top end cap; 5. Bottom end cap; 6. Sample platform; 7. X / Y axis displacement adjuster; 8. Vacuum connection port; 9. Liquid nitrogen inlet / outlet pipe; 10. Upper platform; 11. Flow channel plug; 12. Lower cap; 13. Light transmission hole; 14. Upper plate; 15. Lower plate; 16. Semi-circular ring stage; 17. Light transmission window; 18. Cap viewing window; 19. X-axis adjusting rod; 20. X-axis adjusting slider; 21. Y-axis adjusting rod; 22. Y-axis adjusting slider; 23. X / Y axis sealing ring; 24. Slide rail; 25. Displacement pressure ring; 26. Liquid nitrogen flow channel; 27. Temperature measuring port; 29. ​​Cable outlet; 30. Handwheel; 31. Vacuum head; 32. Vacuum core. Detailed Implementation

[0030] This invention discloses a temperature-controllable vacuum stage, comprising a stage shell 1, a fixing device 2, a stage cap 3, a top end cap 4, a bottom end cap 5, a sample platform 6, an X / Y axis displacement adjuster 7, and two vacuum connection ports 8. This invention enables the observation of microscopic changes in samples during cooling, heating, and temperature control under vacuum or non-vacuum conditions, with high temperature control accuracy. The overall structure is simple, easy to install, and convenient to operate.

[0031] The purpose of this invention is to provide a temperature-controllable vacuum stage for determining the collapse temperature of freeze-dried products. This stage allows for precise temperature control, with sealed connections for all components, excellent overall sealing, and quick alignment with the light-transmitting aperture 13. It also features an X / Y axis displacement adjuster 7 for easy adjustment of the observation area, convenient installation and fixation, and easy sample loading. The liquid nitrogen flow rate and electric heating power within the sample platform 6 are controlled by a temperature probe installed inside the platform, thereby achieving temperature rise, fall, and constant temperature control on the surface of the sample platform 6.

[0032] The sample platform 6 includes a liquid nitrogen inlet / outlet pipe 9, an upper platform 10, a flow channel plug 11, and a lower cover 12. One end of the liquid nitrogen inlet / outlet pipe 9 is connected to the two openings on the outside of the upper platform 10 and communicates with the liquid nitrogen flow channel 26 inside the upper platform 10. The other end passes through the opening of the top end cover 4 and connects to the external liquid nitrogen inlet / outlet pipe 9. A liquid nitrogen flow channel 26 is provided on the lower side of the upper platform 10, which can fit with the flow channel plug 11. The upper platform 10 has a temperature measuring port 27, an electric heating fixing port, and a wire outlet 29. The annular electric heating is fixed by the interference fit between the upper platform 10 and the lower cover 12. The centers of the light-transmitting holes of the upper platform 10 and the lower cover 12 are aligned.

[0033] Vacuum connection ports 8 are installed on both sides of the stage housing 1. One is connected to a vacuum pump to evacuate the stage and create a vacuum environment inside the stage cavity; the other is connected to a vacuum gauge to read the vacuum level inside the stage cavity.

[0034] The stage housing 1 has a positioning device and a light-transmitting window at the bottom, which can be mounted on a microscope. The sample observation area can be adjusted by the X / Y axis displacement adjuster 7, and the sample can be observed through the viewing window above the stage cover 3.

[0035] The stage housing 1 includes an upper plate 14 and a lower plate 15. The stage housing 1 is placed on the microscope stage. The fixing device 2 located below the stage housing 1 is adjusted to align the center of the microscope light source and the light transmission window 17 on the lower side of the stage housing 1. A semi-circular stage 16 is provided on the lower plate 15 to position the sample platform 6, so that the light transmission hole 13 of the sample platform 6 is aligned with the center of the light transmission window 17 of the lower plate 15. The stage cap 3 can be screwed onto the upper plate 14, and the viewing window 18 of the cap is aligned with the center of the light transmission hole 13 of the sample platform 6. One end of the stage housing 1 is connected to the top end cap 4, and the other end is connected to the bottom end cap 5.

[0036] The top end cap 4 has liquid nitrogen inlet and outlet and aviation plug. The electric heating power cord and temperature probe signal line in the sample platform 6 can be connected to external equipment through the aviation plug.

[0037] The X / Y axis displacement adjuster 7 includes an X-axis adjusting rod 19, an X-axis adjusting slider 20, a Y-axis adjusting rod 21, a Y-axis adjusting slider 22, an X / Y axis sealing ring 23, a slide rail 24, and a displacement pressure ring 25. The observation area of ​​the microscope is adjusted by moving the sample within the displacement pressure ring 25 using the handwheels 30 on the X-axis adjusting rod 19 and the Y-axis adjusting rod 21.

[0038] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0039] like Figure 1 , 2 As shown, the present invention mainly includes a stage housing 1, a fixing device 2 disposed under the stage housing 1, a stage screw cap 3 disposed on the stage housing 1, a top end cap 4 disposed at the top of the stage housing 1, a bottom end cap 5 disposed at the bottom of the stage housing 1, a sample platform 6 disposed inside the stage housing 1, an X / Y axis displacement adjuster 7 connected to the stage housing 1, and two vacuum connection ports 8 connected to both sides of the stage housing 1.

[0040] like Figure 1-5 As shown, each component connection is equipped with a sealing device.

[0041] like Figure 6 , 7As shown, the sample platform 6 includes liquid nitrogen inlet and outlet pipes 9, upper platform 10, flow channel plug 11, and lower cap 12.

[0042] like Figure 6 , 7 As shown, the stage housing 1 includes an upper plate 14, a lower plate 15, and a semi-circular ring stage 16.

[0043] like Figure 10 As shown, the X / Y axis displacement adjuster 7 includes an X-axis adjusting rod 19, an X-axis adjusting slider 20, a Y-axis adjusting rod 21, a Y-axis adjusting slider 22, an X / Y axis sealing ring 23, a slide rail 24, and a displacement pressure ring 25.

[0044] like Figure 1 , 2 As shown in Figures 8 and 9, the fixing device 2 can adjust the position of the stage housing 1 on the microscope stage so that the light window 17 on the stage housing 1 is aligned with the center of the microscope light source.

[0045] like Figure 1 , 2 As shown, the sample platform 6 is placed inside the stage shell 1, and the semi-circular ring stage 16 limits the sample platform 6. The center is aligned with the light window 17, the screw cap viewing window 18 and the light hole 13 of the sample platform 6 on the lower plate 15.

[0046] like Figure 1 , 2 As shown in Figures 6 and 7, one end of the liquid nitrogen inlet / outlet pipe 9 is connected to the liquid nitrogen flow tank 26 inside the upper platform 10, and the other end passes through the opening of the top end cap 4 to connect to the external liquid nitrogen control system. The opening is sealed with a sealing ring.

[0047] like Figure 6 , 7 As shown, a liquid nitrogen flow channel 26 is provided on the lower side of the upper platform 10, and the liquid nitrogen flow channel 26 is in contact with the flow channel plug 11.

[0048] like Figure 6 , 7 As shown, the upper platform 10 and the lower cover 12 are interference-fitted to fix the annular electric heater inside the upper platform 10.

[0049] like Figure 6 , 7 As shown, the upper platform 10 and the lower cover 12 are aligned at the center.

[0050] like Figure 6 , 7 As shown, the upper platform 10 has a flat surface, allowing samples to be placed on it.

[0051] like Figure 6 , 7As shown, the upper platform 10 has a temperature measuring port 27, a ring-shaped electric heating fixing port, and a cable outlet 29. The temperature probe is inserted into the temperature measuring port 27 to measure the temperature of the upper platform 10. The temperature probe signal line and the ring-shaped electric heating power line are connected from the cable outlet 29 to the aviation plug at the top end cover 4, and then connected to the external control equipment.

[0052] like Figure 6 , 7 As shown, the liquid nitrogen flow rate and annular electric heating power within the sample platform 6 are controlled by a temperature probe installed inside the sample platform 6, thereby achieving cooling, heating, and constant temperature control of the surface of the sample platform 6.

[0053] like Figure 8 , 9 As shown, the stage housing 1 has vacuum connection ports 8 on both sides. One port is connected to a vacuum pump to evacuate the stage and create a vacuum environment inside the stage cavity; the other port is connected to a vacuum gauge to read the vacuum level inside the stage cavity.

[0054] like Figure 11 As shown, the X-axis adjusting rod 19 and the Y-axis adjusting rod 21 are composed of a handwheel 30, a vacuum head 31, a vacuum core 32, and an X / Y axis sealing ring 23.

[0055] like Figure 10 As shown, the X-axis adjusting slider 20, the Y-axis adjusting slider 22, and the slide rail 24 are connected by a wedge structure.

[0056] like Figure 1 , 2 As shown, the displacement ring 25 is connected to the Y-axis adjusting slider 22, the displacement ring 25 is in contact with the upper surface of the upper platform 10, and the movement range of the displacement ring 25 in the X / Y direction is from the center of the upper platform 10 to the edge of the upper platform 10.

[0057] like Figure 10 , 11 As shown, by rotating the handwheel 30 on the X-axis adjusting rod 19 and the Y-axis adjusting rod 21, the X-axis adjusting slider 20 and the Y-axis adjusting slider 22 are moved, causing the displacement pressure ring 25 and its internal fragments to move on the surface of the upper platform 10, thereby adjusting the observation area of ​​the microscope.

[0058] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A temperature-controllable vacuum stage, characterized in that, The system includes a stage housing (1), a fixing device (2) disposed under the stage housing (1), a stage screw cap (3) disposed on the stage housing (1), a top end cap (4) disposed at the top of the stage housing (1), a bottom end cap (5) disposed at the bottom of the stage housing (1), a sample platform (6) disposed inside the stage housing (1), an X / Y axis displacement adjuster (7) connected to the stage housing (1), and two vacuum connection ports (8) connected to both sides of the stage housing (1). The liquid nitrogen flow rate and electric heating power inside the sample platform (6) are controlled by a temperature probe installed inside the sample platform (6), thereby achieving heating, cooling and constant temperature control of the surface of the sample platform (6). The sample platform (6) includes a liquid nitrogen inlet / outlet pipe (9) and an upper platform (10). One end of the liquid nitrogen inlet / outlet pipe (9) is connected to the openings at both ends of the outer side of the upper platform (10) and communicates with the liquid nitrogen flow channel (26) inside the upper platform (10). The other end passes through the opening of the top end cap (4) and connects to the external liquid nitrogen inlet / outlet pipe (9). The sample platform (6) is provided with a flow channel plug (11). The liquid nitrogen flow channel (26) is left on the lower side of the upper platform (10). The liquid nitrogen flow channel (26) fits against the flow channel plug (11). The stage housing (1) includes an upper plate (14) and a lower plate (15). The stage housing (1) is placed on the microscope stage. The fixing device (2) located below the stage housing (1) is adjusted so that the center of the microscope light source and the light transmission window (17) on the lower side of the stage housing (1) are aligned. A semi-circular ring stage (16) is provided on the lower plate (15) to position the sample platform (6) so that the light transmission hole (13) of the sample platform (6) is aligned with the center of the light transmission window (17) of the lower plate (15). The stage cap (3) can be screwed onto the upper plate (14). The sample is observed through the cap viewing window (18) above the stage cap (3). The cap viewing window (18) is aligned with the center of the light transmission hole (13) of the sample platform (6). The X / Y axis displacement adjuster (7) includes an X-axis adjusting rod (19), an X-axis adjusting slider (20), a Y-axis adjusting rod (21), a Y-axis adjusting slider (22), an X / Y axis sealing ring (23), a slide rail (24), and a displacement pressure ring (25). The X-axis adjusting rod (19) and the Y-axis adjusting rod (21) are composed of a handwheel (30), a vacuum head (31), a vacuum core (32), and the X / Y axis sealing ring (23). The X-axis adjusting slider (20), the Y-axis adjusting slider (22), and the slide rail (25) are also composed of a handwheel (30), a vacuum head (31), a vacuum core (32), and the X / Y axis sealing ring (23). 24) are connected by a wedge structure. The displacement ring (25) is connected to the Y-axis adjusting slider (22). The displacement ring (25) is attached to the upper surface of the upper platform (10). The displacement ring (25) moves from the center of the upper platform (10) to the edge of the upper platform (10) in the X / Y direction. The sample in the displacement ring (25) is moved by adjusting the handwheel (30) on the X-axis adjusting rod (19) and the Y-axis adjusting rod (21), thereby adjusting the observation area of ​​the microscope.

2. The temperature-controllable vacuum stage according to claim 1, characterized in that, The upper platform (10) has a temperature measuring port (27), an electric heating fixing port and a cable outlet (29).

3. A temperature-controllable vacuum stage according to claim 2, characterized in that, The sample platform (6) also includes a lower cover (12); the light-transmitting holes of the upper platform (10) and the lower cover (12) are aligned.

4. A temperature-controllable vacuum stage according to claim 1, characterized in that, One of the two vacuum connection ports (8) is connected to a vacuum pump to evacuate the stage and create a vacuum environment inside the stage cavity; the other is connected to a vacuum gauge to read the vacuum level inside the stage cavity.

5. A temperature-controllable vacuum stage according to claim 1, characterized in that, The top end cap (4) has a liquid nitrogen inlet / outlet and an aviation plug. The electric heating power line and temperature probe signal line in the sample platform (6) are connected to external equipment through the aviation plug.

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