A frozen sample holder for transmission electron microscope

Abstract

The present invention discloses a transmission electron microscope freezing sample rod, comprising a handle, a rod shaft, a rod head, a liquid nitrogen storage device and a liquid nitrogen inlet and outlet pipeline; wherein the rod shaft connects the rod head and the handle; the liquid nitrogen storage device is arranged in the handle; the liquid nitrogen inlet and outlet pipeline is used to control the flow direction of liquid nitrogen in the transmission electron microscope freezing sample rod, and an inlet and a first outlet and a second outlet are arranged on the handle; the flow direction of liquid nitrogen during refrigeration: liquid nitrogen flows in from the inlet, directly flows into the rod shaft, is split in the rod shaft, a part of it flows into the rod head through the rod shaft, and then flows back from the rod head and flows out from the first outlet; the other part flows back from the rod shaft to the liquid nitrogen storage device, and flows out from the second outlet via the liquid nitrogen storage device; the second outlet is controlled by a fluid valve. The present invention can realize rapid refrigeration and low-temperature maintenance of samples placed on the rod head by optimizing the pipeline arrangement of liquid nitrogen, with high efficiency and high controllability.

Description

Technical Field

[0001] The invention relates to the field of transmission electron microscope sample rods, and in particular to a transmission electron microscope freezing sample rod. Background Art

[0002] At present, the frozen sample rod of transmission electron microscope usually adopts the method of cooling the metal by liquid nitrogen and cooling the sample rod by metal. This method is inefficient, has a long cooling time, low efficiency and poor controllability. Similarly, after cooling, the heating time is long, the efficiency is low and the controllability is poor. Summary of the invention

[0003] In view of the above-mentioned defects of the prior art, an object of the present invention is to provide a transmission electron microscope freezing sample rod, which can achieve rapid refrigeration and low temperature maintenance and has high efficiency and high controllability.

[0004] To achieve the above-mentioned purpose, the present invention provides a transmission electron microscope freezing sample rod, comprising a handle, a rod body, a rod head, a liquid nitrogen storage device and a liquid nitrogen inlet and outlet pipeline;

[0005] One end of the shaft is connected to the shaft head, and the other end of the shaft is fixedly connected to the handle;

[0006] The liquid nitrogen storage device is disposed in the handle;

[0007] The liquid nitrogen inlet and outlet pipe is used to control the flow direction of liquid nitrogen in the transmission electron microscope freezing sample rod. An inlet and a first outlet and a second outlet are arranged on the handle. During refrigeration, the liquid nitrogen flows in from the inlet and directly into the rod shaft, and is divided at the rod shaft. A part of the liquid nitrogen flows into the rod head through the rod shaft, and then flows back from the rod head and flows out from the first outlet. Another part flows back from the rod shaft to the liquid nitrogen storage device and flows out from the second outlet via the liquid nitrogen storage device. The second outlet is controlled by a fluid valve.

[0008] Further, the shaft comprises a first shaft and a second shaft connected to each other, the head of the first shaft is connected to the base of the second shaft; the base of the first shaft is fixedly connected to the handle; the head of the second shaft is fixedly connected to the club head;

[0009] The liquid nitrogen inlet and outlet pipelines include a first pipeline, a second pipeline, a third pipeline and a fourth pipeline;

[0010] The first pipe has one end as the inlet of the liquid nitrogen inlet and outlet pipe, and the other end thereof passes through the liquid nitrogen storage device and directly extends to the head of the first shaft;

[0011] The second pipe is arranged in the shaft, one end of which is connected to the liquid nitrogen storage device; the other end of which extends to the position of the head of the first shaft, so that the liquid nitrogen flows into the liquid nitrogen storage device;

[0012] The third pipeline is used to connect the liquid nitrogen storage device and the second outlet of the liquid nitrogen inlet and outlet pipeline, and the third pipeline is controlled by the fluid valve;

[0013] One end of the fourth conduit is disposed at the head of the first shaft, the fourth conduit extends along the second shaft to the head, folds back inside the head, and reaches the first outlet through the second shaft and the first shaft;

[0014] The diameter of the fourth pipeline is smaller than that of the first pipeline and the second pipeline.

[0015] Furthermore, the liquid nitrogen storage device comprises an inner liner and an outer shell, wherein the inner liner is wrapped in the outer shell, and the outer shell is wrapped in the handle; the end of the third pipe is sealed and connected to the inner liner; the port of the second pipe is sealed and connected to the inner liner; the first pipe is sealed and connected to the inner liner at a position where it penetrates into the inner liner on the inlet side of the liquid nitrogen inlet and outlet pipe; a section of the first pipe that passes through the inner liner and extends to the head of the first shaft is located inside the second pipe, and the liquid nitrogen flows back into the inner liner through the gap between the second pipe and the first pipe.

[0016] Furthermore, the inlet includes a pipe ferrule and a threaded connector, the threaded connector is clamped on the handle, and the pipe ferrule and the threaded connector are threadedly connected to be connected to an external nitrogen supply device.

[0017] Furthermore, the control switch of the fluid valve is a threaded rod, and the opening flow of the fluid valve is adjusted by rotating the threaded rod.

[0018] Furthermore, the rod head is provided with a heating component, which includes a circuit board and a heating chip, and the circuit board is used to control the operation of the heating chip; the heating chip is arranged at the sample carrier of the rod head, and is used to heat the sample placed on the sample carrier, so as to control the sample temperature at an expected temperature.

[0019] Furthermore, the rod head is also provided with a pressure cover and a contact pin, the contact pin is used for the electrical connection between the temperature increasing chip and the circuit board, and the pressure cover is used for fixing the temperature increasing chip on the rod head.

[0020] Compared with the prior art, the transmission electron microscope freezing sample holder of the present invention optimizes the pipeline arrangement of liquid nitrogen so that liquid nitrogen can directly act on the holder head and realizes rapid circulation of liquid nitrogen in the sample holder, thereby realizing rapid refrigeration and low temperature maintenance with high efficiency and controllability. Furthermore, by adding a heating component to the holder head, the accuracy of temperature control can be further improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 is a structural diagram of a frozen sample rod of a preferred embodiment of the present invention;

[0022] Figure 2 yes Figure 1 Exploded diagram of

[0023] Figure 3 yes Figure 1 sectional view of

[0024] Figure 4 yes Figure 1 A partial enlarged view of the club head;

[0025] Figure 5 This is a schematic diagram of the liquid nitrogen pipeline inside the club head. DETAILED DESCRIPTION

[0026] To further illustrate the various embodiments, the present invention provides drawings. These drawings are part of the disclosure of the present invention, which are mainly used to illustrate the embodiments and can be used in conjunction with the relevant descriptions in the specification to explain the operating principles of the embodiments. With reference to these contents, a person of ordinary skill in the art should be able to understand other possible implementations and advantages of the present invention. The components in the figures are not drawn to scale, and similar component symbols are generally used to represent similar components.

[0027] The present invention will now be further described with reference to the accompanying drawings and specific implementation methods.

[0028] Example 1

[0029] like Figure 1 - Figure 5 As shown, the present invention provides a freezing sample rod, including a handle 10, a rod body 20, a rod head 30, a liquid nitrogen storage device 40 and a liquid nitrogen inlet and outlet pipe 50.

[0030] In this embodiment, the shaft 20 includes a first shaft 21, a second shaft 22 and an insulating sleeve 23 which are connected to each other. The head of the first shaft 21 is connected to the base of the second shaft 22 and is sealed by a sealing ring 25. The base of the first shaft 21 is fixedly connected to the handle. The head of the second shaft 22 is fixedly connected to the club head 30. The insulating sleeve 23 is put on the club head 30 to insulate the club head 30.

[0031] The liquid nitrogen storage device 40 is disposed in the handle 10 and is used to temporarily store a certain amount of liquid nitrogen for temperature control.

[0032] The inlet and outlet of the liquid nitrogen inlet and outlet pipe 50 include an inlet P1, a first outlet P2 and a second outlet P3. The inlet P1, the first outlet P2 and the second outlet P3 are all arranged on the handle 10. When refrigeration is performed, the flow direction of the liquid nitrogen is as follows: the liquid nitrogen flows in from the inlet P1, directly flows into the head of the first shaft 21, is divided at the head of the first shaft 21, a part of it is connected to the head 30 through the second shaft 22, and then flows back from the head 30 and flows out from the first outlet P2; the other part flows back from the first shaft 21 to the liquid nitrogen storage device 4, and flows out from the second outlet P3 through the liquid nitrogen storage device 4. The second outlet P3 is controlled by the fluid valve 55. The diameter of the first outlet P2 is smaller than the diameter of the second outlet P3.

[0033] In this embodiment, specifically, the liquid nitrogen inlet and outlet pipeline 50 includes a first pipeline 51, a second pipeline 52, a third pipeline 53 and a fourth pipeline 54;

[0034] A first pipe 51, one end of which is connected to the inlet P1 of the liquid nitrogen inlet and outlet pipe, and the other end of which passes through the inner liner 41 and directly extends to the head of the first shaft 21;

[0035] The second pipe 52 is disposed in the shaft 20, one end of which is connected to the liquid nitrogen storage device 4; the other end of the second pipe 52 extends to the position of the head of the first shaft 21, so that the liquid nitrogen flows into the liquid nitrogen storage device 4;

[0036] The third pipeline 53 is used to connect the liquid nitrogen storage device 4 and the second outlet P3 of the liquid nitrogen inlet and outlet pipeline 50 . The third pipeline 53 is controlled by a fluid valve 55 .

[0037] One end of the fourth pipe 54 is disposed at the head of the first shaft 21 , and the fourth pipe 54 extends along the second shaft 22 to the club head 30 , turns back inside the club head 30 , and reaches the first outlet P2 of the liquid nitrogen inlet and outlet pipe 5 located at the handle 10 through the second shaft 22 and the first shaft 21 .

[0038] Preferably, the liquid nitrogen storage device 40 includes an inner liner 41, an outer shell 42, 43, the inner liner is wrapped in the outer shell 42, 43, and the outer shell 42, 43 is assembled into one and further wrapped in the handle 10; the end of the third pipe 53 is sealed and connected to the inner liner 41; the port of the second pipe 52 is sealed and connected to the inner liner 41 through a sealing ring 24; the first pipe 51 penetrates into the inner liner 41 at the inlet side of the liquid nitrogen inlet and outlet pipe 50, and is sealed and connected to the inner liner 41; the section of the first pipe 51 extending from the inner liner 41 to the head of the first shaft 21 is located inside the second pipe 52, and the liquid nitrogen flows back to the inner liner 41 through the gap between the second pipe 52 and the first pipe 51.

[0039] Preferably, the inlet P1 is composed of a tube ferrule 56 and a threaded connector 57, the tube ferrule 56 and the threaded connector 57 are threadedly connected, the threaded connector 57 is clamped on the handle 10, and is connected to an external liquid nitrogen supply device through the tube ferrule 56.

[0040] Preferably, the control switch of the fluid valve 55 is a threaded rod, and the opening flow of the fluid valve 55 is adjusted by rotating the threaded rod, so that the liquid nitrogen flow rate can be accurately controlled.

[0041] Preferably, Figure 1 - Figure 3 As shown, for the convenience of production, the handle 10 includes a front shell 12, a rear shell 13, and hoops 11 and 14. The front shell 12 and the rear shell 13 cooperate to form a closed cavity, and the two ends thereof are fastened by hoops 11 and 14 respectively.

[0042] like Figure 4 As shown, in this embodiment, preferably, in order to further accurately control the temperature of the sample, a heating component is provided on the rod head 30. Specifically, the heating component includes a circuit board 31, a heating chip 32 and a contact pin 34. The heating chip 32 is placed in a groove on the rod head 30, which is the sample carrier area of ​​the rod head 30. The circuit board 31 is led out from the rod body 20. The electrodes of the heating chip 32 and the circuit board 31 are electrically connected through the contact pin 34. A pressure cap 33 is provided on the rod head 30. The pressure cap 33 is used to fix the contact pin 34 and the heating chip 32, thereby fixing the circuit connection between the circuit board 31 and the heating chip 32. In the structure of this embodiment, the position of the heating chip 32 is the sample carrier of the rod head 30. The sample can be directly placed on the heating chip 32. After the heating chip 32 is powered on, the sample is heated and the ambient temperature of the sample is controlled to a desired temperature. An electrical socket 15 is provided on the handle 10, and the circuit board 31 can be powered by the electrical socket 15. Preferably, the electrical plug is an aviation socket, which can provide a stable and reliable electrical connection.

[0043] Working principle:

[0044] The sample is placed on the rod head 30 of the freezing sample rod. When refrigerating, the fluid valve 55 is opened, and liquid nitrogen enters from the inlet P1, flows into the rod head 30 through the first pipe 51 and the fourth pipe 54 to quickly refrigerate the rod head 30 and the sample on the rod head, and then flows out from the first outlet P2; at the same time, the liquid nitrogen also flows to the inner liner 41 through the first pipe 51, and then flows out from the second outlet P3 after passing through the fluid valve 55 from the inner liner 41, clearing the hot air in the shaft 20 (relative to the temperature of the liquid nitrogen), and storing part of the liquid nitrogen in the inner liner 41. After the refrigeration effect is achieved, the fluid valve 55 and the liquid nitrogen supply are closed, and the liquid nitrogen in the inner liner 41 is used for heat preservation, and the liquid nitrogen in the inner liner 41 flows out through the fourth pipe 54 to maintain the temperature of the sample on the rod head 30.

[0045] Controlling the temperature of the sample by controlling the flow rate of liquid nitrogen to control the refrigeration capacity will have a certain hysteresis effect. In this embodiment, in order to quickly and accurately control the temperature of the sample, auxiliary heating control can be performed by the heating component arranged on the rod head 30, so that the temperature of the sample is controlled within a suitable temperature range.

[0046] Compared with the prior art, the transmission electron microscope freezing sample holder of the present invention optimizes the pipeline arrangement of liquid nitrogen so that liquid nitrogen can directly act on the holder head and realizes rapid circulation of liquid nitrogen in the sample holder, thereby realizing rapid refrigeration and low temperature maintenance with high efficiency and controllability. Furthermore, by adding a heating component to the holder head, the temperature of the sample can be quickly and accurately controlled.

[0047] Although the present invention has been specifically shown and described in conjunction with the preferred embodiments, it should be understood by those skilled in the art that various changes may be made to the present invention in form and details without departing from the spirit and scope of the present invention as defined by the appended claims, all of which are within the scope of protection of the present invention.

Claims

1. A transmission electron microscope freezing sample holder, comprising a handle, a holder, a holder head, a liquid nitrogen storage device and a liquid nitrogen inlet and outlet pipe; characterized in that: One end of the shaft is connected to the shaft head, and the other end of the shaft is fixedly connected to the handle; The liquid nitrogen storage device is disposed in the handle; The liquid nitrogen inlet and outlet pipe is used to control the flow direction of liquid nitrogen in the transmission electron microscope freezing sample rod. An inlet and a first outlet and a second outlet are arranged on the handle. During refrigeration, the liquid nitrogen flows in from the inlet and directly into the rod shaft, and is divided at the rod shaft. A part of the liquid nitrogen flows into the rod head through the rod shaft, and then flows back from the rod head and flows out from the first outlet. The other part flows back in the rod shaft to the liquid nitrogen storage device, and flows out from the second outlet via the liquid nitrogen storage device. The second outlet is controlled by a fluid valve.

2. The frozen sample holder for transmission electron microscopy according to claim 1, characterized in that: The shaft comprises a first shaft and a second shaft connected to each other, the head of the first shaft is connected to the base of the second shaft; the base of the first shaft is fixedly connected to the handle; the head of the second shaft is fixedly connected to the club head; The liquid nitrogen inlet and outlet pipelines include a first pipeline, a second pipeline, a third pipeline and a fourth pipeline; The first pipe has one end as the inlet of the liquid nitrogen inlet and outlet pipe, and the other end thereof passes through the liquid nitrogen storage device and directly extends to the first shaft head; The second pipe is arranged in the shaft, one end of which is connected to the liquid nitrogen storage device; the other end of which extends to the position of the head of the first shaft, so that the liquid nitrogen flows into the liquid nitrogen storage device; The third pipeline is used to connect the liquid nitrogen storage device and the second outlet of the liquid nitrogen inlet and outlet pipeline, and the third pipeline is controlled by the fluid valve; One end of the fourth conduit is disposed at the head of the first shaft, the fourth conduit extends along the second shaft to the head, folds back inside the head, and reaches the first outlet through the second shaft and the first shaft; The diameter of the fourth pipeline is smaller than that of the first pipeline and the second pipeline.

3. The frozen sample holder for transmission electron microscopy according to claim 2, characterized in that: The liquid nitrogen storage device comprises an inner liner and an outer shell, wherein the inner liner is wrapped in the outer shell, and the outer shell is wrapped in the handle; the end of the third pipe is sealed and connected to the inner liner; and the port of the second pipe is sealed and connected to the inner liner.

4. The frozen sample holder for transmission electron microscopy according to claim 3, characterized in that: The first pipe penetrates into the inner liner at the inlet side of the liquid nitrogen inlet and outlet pipe and is sealed and connected to the inner liner; a section of the first pipe extending from the inner liner to the head of the first shaft is located inside the second pipe, and the liquid nitrogen flows back into the inner liner through the gap between the second pipe and the first pipe.

5. The frozen sample holder for transmission electron microscopy according to claim 1, characterized in that: The inlet comprises a pipe ferrule and a threaded connector, the threaded connector is clamped on the handle, and the pipe ferrule is threadedly connected to the threaded connector for connection with an external nitrogen supply device.

6. The frozen sample holder for transmission electron microscopy according to claim 1, characterized in that: The control switch of the fluid valve is a threaded rod, and the opening flow of the fluid valve is adjusted by rotating the threaded rod.

7. The frozen sample holder for transmission electron microscopy according to claim 1, characterized in that: The rod head is provided with a heating component, which includes a circuit board and a heating chip. The circuit board is used to control the operation of the heating chip. The heating chip is arranged at the sample carrier of the rod head and is used to heat the sample placed on the sample carrier to control the sample temperature at the expected temperature.

8. The frozen sample holder for transmission electron microscopy according to claim 7, characterized in that: The rod head is also provided with a pressure cover and a contact pin, wherein the contact pin is used for the electrical connection between the temperature increasing chip and the circuit board, and the pressure cover is used for fixing the temperature increasing chip on the rod head.

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