Liquid nitrogen holding device for scanning electron microscope low temperature frozen brittle fracture sample

CN224719964UActive Publication Date: 2026-09-04HANGZHOU YANQU INFORMATION TECH CO LTD
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Patent Information

Application Number
CN202521893647.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-09-03
Publication Date
2026-09-04
Estimated Expiration
2035-09-03

AI Technical Summary

Technical Problem

[0006]2.回收时造成污染

Benefits of technology

[0023]本实用新型提供了一种用于扫描电子显微镜低温冷冻脆断制样的液氮盛装装置,通过设置上窄下宽的座体,提高了座体的稳固性,从而使得其使用时稳定性较高,不容易被打翻,进而提高了作业安全性。并且,在座体的容纳槽的槽底开设有不同结构的盛装槽,用于盛装不同形状的样品,这样设置不仅提高了该液氮盛装装置的适配性,无需手工夹持,而且在进行脆断时,液氮放置时仅需高于容纳槽的槽底即可,减少了单次液氮使用量,提高了液氮利用率,避免浪费;然后将需要脆断的样品放置于对应盛装槽,也可同步对多种样品同时进行脆断,作业效率更高。

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Abstract

The utility model belongs to low temperature freezing brittle fracture technical field discloses a kind of liquid nitrogen containing device for scanning electron microscope low temperature freezing brittle fracture sample preparation. The liquid nitrogen containing device for scanning electron microscope low temperature freezing brittle fracture sample preparation includes seat body, and seat body is the structure of upper narrow lower wide;The top of seat body is equipped with accommodating groove;The groove bottom of accommodating groove is equipped with multiple containing grooves, and at least part of multiple containing grooves is different in structure, to make at least part in multiple containing grooves be used for containing different shape sample respectively. Its single liquid nitrogen usage is less, and liquid nitrogen utilization rate is high, without manual clamping, liberate labor, improve operating efficiency;And container high stability, safety can be improved.
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Description

Technical Field

[0001] This utility model relates to the field of cryogenic freezing brittle fracture technology, and in particular to a liquid nitrogen container for cryogenic freezing brittle fracture sample preparation for scanning electron microscopy. Background Technology

[0002] Scanning Electron Microscope (SEM) cryogenic freezing and brittle fracture sample preparation technology is a method of preserving water-containing or electron beam-sensitive samples by cryogenic freezing, mainly used in fields such as biology and polymer materials.

[0003] Currently, liquid nitrogen brittle fracture is commonly used for cryogenic brittle fracture sample preparation. Liquid nitrogen brittle fracture is a key sample pretreatment technique in SEM (Scanning Electron Microscopy) sample preparation, especially suitable for materials requiring observation of internal structure or cleaning of the fracture surface, such as polymers (e.g., PE, PP, rubber, epoxy resin), composite materials (e.g., carbon fiber / resin-based, multilayer coatings), and coatings. During use, liquid nitrogen (temperature -196℃ at standard atmospheric pressure) instantly embrittles the material, reducing plastic deformation during fracture and avoiding tearing, burrs, or thermal damage caused by conventional cutting. The fracture surface clearly reveals the internal phase distribution, porosity, fiber orientation, and other characteristics of the material, avoiding artifacts introduced by mechanical polishing or ion abrasion.

[0004] Before using liquid nitrogen brittle fracture technology to process samples, the liquid nitrogen in the liquid nitrogen container needs to be removed and poured into a specific container. Since there are no dedicated containers for liquid nitrogen brittle fracture on the market, containers used for transferring or storing liquid nitrogen are generally used as substitutes. Currently usable containers generally include insulated cups, metal boxes, bowls, and jugs. However, directly using these containers to hold liquid nitrogen has the following disadvantages:

[0005] 1. Waste of liquid nitrogen resources. The containers mentioned above are all too large, requiring a large amount of liquid nitrogen to be poured in each time for normal use. For example, with a cup-shaped container, the volume of liquid nitrogen needs to be almost to the rim, requiring 300-500ml each time. In this case, the sample needs to be held with tweezers and immersed in liquid nitrogen to achieve the desired effect.

[0006] 2. Pollution during recycling. Failure to recycle such containers after liquid nitrogen freezing and brittle fracture will result in resource waste. However, recycling them will contaminate the remaining liquid nitrogen due to impurities present after use.

[0007] 3. Low efficiency and inconvenient to use. In some cases, when liquid nitrogen breaks samples, the immersion time in liquid nitrogen can range from 2-3 minutes to 10-15 minutes. Because the liquid nitrogen container is too large, it is inconvenient to retrieve the sample after it has been placed in. Tweezers must be used to hold the sample in place while waiting, which is time-consuming and laborious.

[0008] 4. Safety risks exist. Because liquid nitrogen containers are too tall and not very stable, there is a risk of tipping over during operation, which may cause injury to operators. If the container tipps over, liquid nitrogen will splash out and come into contact with a large amount of skin, causing severe frostbite.

[0009] Therefore, there is an urgent need for a liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy to solve the above-mentioned technical problems. Utility Model Content

[0010] The purpose of this invention is to provide a liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy. This device can reduce the amount of liquid nitrogen used per batch, improve utilization, and eliminate the need for manual clamping, thus freeing up labor and improving work efficiency. In addition, the container has high stability and improved safety.

[0011] To achieve this objective, the present invention adopts the following technical solution:

[0012] A liquid nitrogen container for cryogenic freezing and fracturing sample preparation for scanning electron microscopy includes a base, which has a structure that is narrower at the top and wider at the bottom; a receiving groove is provided on the top of the base; and multiple holding slots are provided on the bottom of the receiving groove, at least some of the multiple holding slots having different structures, so that at least some of the multiple holding slots are used to hold samples of different shapes.

[0013] Optionally, the plurality of the above-mentioned containers are configured as at least one first container, at least one second container, at least one third container, and at least one fourth container, wherein the first container, the second container, the third container, and the fourth container have different structures.

[0014] Optionally, the first container is cylindrical and is used to hold strip-shaped or columnar samples; the second container is arc-shaped and is used to hold block-shaped or granular samples; the third container is arc-shaped and is used to hold arc-shaped samples; and the fourth container is rectangular and is used to hold flat, sheet-shaped samples.

[0015] Optionally, the third and fourth containers are interconnected, and the maximum distance between the bottom of the third container and the bottom of the receiving tank in the vertical direction is A, and the distance between the bottom of the fourth container and the bottom of the receiving tank in the vertical direction is B, where A > B.

[0016] Optionally, there are four first containers evenly distributed, and a third container is opened between two of the first containers arranged diagonally in one group, and a fourth container is opened between two of the first containers arranged diagonally in another group.

[0017] Optionally, there are four second containers evenly distributed, and each of the second containers is disposed between two adjacent first containers.

[0018] Optionally, the aforementioned base is a frustum-shaped structure that is narrower at the top and wider at the bottom, or a frustum-shaped structure.

[0019] Optionally, the aforementioned base can be a stainless steel base, a glass base, an aluminum alloy base, or a polytetrafluoroethylene base.

[0020] Optionally, the cross-sectional area of ​​the receiving groove gradually decreases from the top to the bottom of the aforementioned seat.

[0021] Optionally, the top of the aforementioned base is also provided with several hanging parts for hanging working tools.

[0022] The beneficial effects of this utility model are:

[0023] This invention provides a liquid nitrogen container for cryogenic brittle fracture sample preparation in scanning electron microscopy. By designing a base that is narrower at the top and wider at the bottom, the stability of the base is improved, resulting in higher stability during use and reducing the risk of tipping over, thus enhancing operational safety. Furthermore, the bottom of the receiving groove in the base has various storage slots to hold samples of different shapes. This design not only improves the adaptability of the liquid nitrogen container, eliminating the need for manual clamping, but also reduces the amount of liquid nitrogen used per batch, increasing utilization and avoiding waste, as the liquid nitrogen only needs to be above the bottom of the receiving groove during brittle fracture. The sample to be brittle fractured is then placed in the corresponding storage slot, allowing for simultaneous brittle fracture of multiple samples, further increasing operational efficiency. Attached Figure Description

[0024] Figure 1 This is an isometric view of a liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy, provided in a specific embodiment of this utility model.

[0025] Figure 2 This is a top view of the liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy, provided in a specific embodiment of this utility model.

[0026] Figure 3 This is a cross-sectional view of a liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy, provided in a specific embodiment of this utility model.

[0027] In the picture:

[0028] 10. Base; 101. Receiving slot; 102. First holding slot; 103. Second holding slot; 104. Third holding slot; 105. Fourth holding slot;

[0029] 20. Hanging and taking department. Detailed Implementation

[0030] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present invention and not intended to limit it. Furthermore, it should be noted that, for ease of description, the accompanying drawings show only the parts relevant to the present invention, not the entire structure.

[0031] In the description of this utility model, unless otherwise explicitly specified and limited, the terms "connected," "linked," and "fixed" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0032] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0033] In the description of this embodiment, the terms "upper," "lower," "left," "right," etc., refer to the orientation or positional relationship shown in the accompanying drawings. They are used only for ease of description and simplification of operation, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model. In addition, the terms "first" and "second" are only used for distinction in description and have no special meaning.

[0034] This embodiment provides a liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation in scanning electron microscopy. It holds liquid nitrogen and accommodates the brittle fracture of the sample. It uses a small amount of liquid nitrogen per batch, has a high liquid nitrogen utilization rate, eliminates the need for manual clamping, freeing up labor and improving operational efficiency; furthermore, the container has high stability, enhancing safety.

[0035] Please refer to Figures 1 to 3Specifically, the liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy includes a base 10, which has a structure that is narrow at the top and wide at the bottom; a receiving groove 101 is provided on the top of the base 10; a plurality of holding slots are provided on the bottom of the receiving groove 101, and at least some of the holding slots have different structures so that at least some of the holding slots are used to hold samples of different shapes.

[0036] During the operation, liquid nitrogen is placed in the receiving tank 101 of the base 10 until it covers the bottom of the receiving tank 101. Then, using tweezers or other operating tools, samples of various shapes such as strips, columns, blocks, granules, arcs, and flat sheets are placed into their corresponding holding tanks. Multiple samples can also be placed into their respective holding tanks. Then, brittle fracture is performed. After a certain period of brittle fracture, the samples are removed with tweezers and cut with operating tools such as scalpels or scissors, or they can be cut directly in the holding tank. This completes the liquid nitrogen brittle fracture of the samples.

[0037] The liquid nitrogen container for cryogenic brittle fracture sample preparation for scanning electron microscopy in this embodiment features a base 10 that is narrower at the top and wider at the bottom, which improves the stability of the base 10 and makes it less prone to tipping over, thus enhancing operational safety. Furthermore, the bottom of the receiving groove 101 of the base 10 has different structured storage slots for holding samples of different shapes. This design not only improves the adaptability of the liquid nitrogen container, eliminating the need for manual clamping, but also allows for liquid nitrogen to be placed only above the bottom of the receiving groove 101 during brittle fracture, reducing the amount of liquid nitrogen used per batch, improving liquid nitrogen utilization, and avoiding waste. The sample to be brittle fractured is then placed in the corresponding storage slot, allowing for simultaneous brittle fracture of multiple samples, resulting in higher operational efficiency.

[0038] Optionally, the base 10 can be a frustum-shaped structure that is narrower at the top and wider at the bottom, which can satisfy its stable structure of being narrower at the top and wider at the bottom.

[0039] Optionally, the base 10 can be made of stainless steel, glass, aluminum alloy, or polytetrafluoroethylene. That is, it can be made of stainless steel, aluminum alloy, or polytetrafluoroethylene, all of which meet the requirements for containing liquid nitrogen.

[0040] For example, the seat 10 in this embodiment is made of stainless steel, such as 304 stainless steel or 316 stainless steel. The seat 10 made of stainless steel has good low temperature resistance, maintains strength and toughness at -196℃, has good corrosion resistance, and is not easily reacted with liquid nitrogen or other chemicals.

[0041] Optionally, the dimensions of the base 10 can be set according to actual needs. For example, in this embodiment, the base 10 is a frustum structure that is narrower at the top and wider at the bottom, with a height of 8cm, a bottom outer diameter of 14cm, a top outer diameter of 12cm, a maximum diameter of 10cm for the receiving groove 101, a depth of 5cm, and a maximum depth of 2cm for the filling groove, which can meet the requirements of the liquid nitrogen filling device for filling samples of various shapes.

[0042] Optionally, the cross-sectional area of ​​the receiving groove 101 gradually decreases from the top to the bottom of the base 10 to form a receiving groove 101 with a wide opening and a narrow bottom, which facilitates the removal of the sample.

[0043] Please refer to Figures 1 to 3 Specifically, the multiple holding slots are configured as at least one first holding slot 102, at least one second holding slot 103, at least one third holding slot 104 and at least one fourth holding slot 105. The first holding slot 102, the second holding slot 103, the third holding slot 104 and the fourth holding slot 105 have different structures, thereby enabling the holding of samples of different shapes.

[0044] More specifically, the first container 102 is cylindrical, i.e., a cylindrical tank, and is used to hold strip-shaped or columnar samples; the second container 103 is arc-shaped, i.e., a partially spherical tank, and is used to hold block-shaped or granular samples; the third container 104 is arc-shaped, i.e., a long arc-shaped tank, and is used to hold arc-shaped samples; the fourth container 105 is rectangular, i.e., a rectangular tank, and is used to hold flat, sheet-shaped samples. This configuration allows for the holding and handling of strip-shaped, columnar, block-shaped, granular, arc-shaped, and flat, sheet-shaped samples, demonstrating high adaptability.

[0045] Of course, if samples of other shapes exist, corresponding container slots can be set up, without specific limitations here.

[0046] The third container 104 is used to hold arc-shaped samples, which can be samples that are arc-shaped themselves, or samples that need to undergo a certain deformation during the brittle fracture process, such as samples that are originally strip-shaped, column-shaped or flat and are transformed into arc-shaped samples through deformation.

[0047] Optionally, the third holding tank 104 and the fourth holding tank 105 are cross-connected. Vertically, the maximum distance between the bottom of the third holding tank 104 and the bottom of the receiving tank 101 is A, and vertically, the distance between the bottom of the fourth holding tank 105 and the bottom of the receiving tank 101 is B, where A > B. This arrangement creates a suspended section in the middle of the flat sample, allowing it to be cut directly within the liquid nitrogen holding device using tools such as scalpels or scissors after the sample has been fractured.

[0048] Specifically, there are four first holding slots 102 evenly distributed. A third holding slot 104 is opened between two diagonally arranged first holding slots 102 in one group, and a fourth holding slot 105 is opened between two diagonally arranged first holding slots 102 in another group. This not only realizes the cross connection between the third holding slot 104 and the fourth holding slot 105, but also realizes the connection between the two and the first holding slots 102. Moreover, the structure is compact and improves the space utilization rate.

[0049] Specifically, there are four second holding slots 103 evenly distributed, and each second holding slot 103 is set between two adjacent first holding slots 102, thereby making better use of the space at the bottom of the holding slot 101 and improving the structural compactness and space utilization.

[0050] Furthermore, the top of the base 10 is provided with several hanging parts 20. These hanging parts 20 are used to hang tools; they protrude from the top of the base 10, forming a raised structure to facilitate the hanging of tools such as tweezers and scissors. Of course, when tools such as scalpels need to be hung, corresponding holes can be made on the handle of the scalpel for hanging. Additionally, this design also functions as a handle, making it convenient to put away and pick up the base 10.

[0051] For example, the top of the seat 10 of this application is provided with two hanging parts 20, which can be used to hang and pick up the working tools, making it convenient to put the seat 10 away.

[0052] Obviously, the above embodiments of this utility model are merely examples for clearly illustrating the present utility model, and are not intended to limit the implementation of the present utility model. Those skilled in the art can make various obvious changes, readjustments, and substitutions without departing from the protection scope of this utility model. It is neither necessary nor possible to exhaustively describe all embodiments here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of this utility model should be included within the protection scope of the claims of this utility model.

Claims

1. A liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy, characterized in that, Includes a base (10), which has a structure that is narrow at the top and wide at the bottom; the top of the base (10) is provided with a receiving groove (101); the bottom of the receiving groove (101) is provided with multiple holding slots, at least some of the multiple holding slots have different structures, so that at least some of the multiple holding slots are used to hold samples of different shapes.

2. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 1, characterized in that, The plurality of the containers are configured as at least one first container (102), at least one second container (103), at least one third container (104) and at least one fourth container (105), wherein the first container (102), the second container (103), the third container (104) and the fourth container (105) have different structures.

3. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 2, characterized in that, The first container (102) is cylindrical and is used to hold strip-shaped or columnar samples; the second container (103) is arc-shaped and is used to hold block-shaped or granular samples; the third container (104) is arc-shaped and is used to hold arc-shaped samples; the fourth container (105) is rectangular and is used to hold flat samples.

4. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 3, characterized in that, The third container (104) and the fourth container (105) are interconnected. The maximum distance between the bottom of the third container (104) and the bottom of the receiving tank (101) in the vertical direction is A. The distance between the bottom of the fourth container (105) and the bottom of the receiving tank (101) in the vertical direction is B. A > B.

5. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 4, characterized in that, The first container (102) is evenly distributed in four places. A third container (104) is opened between two first container (102) arranged diagonally in one group, and a fourth container (105) is opened between two first container (102) arranged diagonally in another group.

6. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 5, characterized in that, There are four second holding slots (103) evenly distributed, and each second holding slot (103) is disposed between two adjacent first holding slots (102).

7. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 1, characterized in that, The base (10) is a frustum structure that is narrow at the top and wide at the bottom, or a frustum structure.

8. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 1, characterized in that, The seat (10) is a stainless steel seat (10), a glass seat (10), an aluminum alloy seat (10), or a polytetrafluoroethylene seat (10).

9. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to claim 1, characterized in that, The cross-sectional area of ​​the receiving groove (101) gradually decreases from the top to the bottom of the seat (10).

10. The liquid nitrogen container for cryogenic freezing and brittle fracture sample preparation for scanning electron microscopy according to any one of claims 1-9, characterized in that, The top of the seat (10) is also provided with several hanging parts (20), which are used to hang working tools.