X-ray photoelectron spectroscopy sample transfer chamber and its transfer method

CN122545562APending Publication Date: 2026-08-11EAST GRP CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-05-08
Publication Date
2026-08-11

AI Technical Summary

Technical Problem

其一,使用商业化的真空转移装置,例如,中国实用新型专利CN210427411U公开了一种用于XPS可回收空气敏感样品的转移装置,包括样品托和样品罩,通过将样品罩2扣置在样品托1上,并且使样品罩2底部的圆形卡槽与环形定位凸台3卡合,采用固定架对样品罩2与样品托1进行固定,将抽真空管5与真空配气系统的管路连接,将样品罩2内的腔室抽为真空状态,之后关闭真空旋塞阀,再取下固定架,然后将装置送入光电子能谱仪的进样室;该类装置虽能实现样品的无空气转移,但存在结构复杂、制造成本高昂的缺陷,难以在各类实验室中普及使用,限制了其应用范围;其二,采用快速转移法,该方法依赖操作人员的操作速度,试图通过缩短转移时间减少空气暴露,但无法从根本上避免样品与空气接触,且对操作人员的熟练度要求极高,操作难度大,同时易因操作差异导致实验数据重复性差,无法满足精准分析的需求

Benefits of technology

[0009]与现有技术相比,本发明的X射线光电子能谱样品转移仓成本低廉且易于普及,相较于现有技术中结构复杂、价格昂贵的商业化真空转移装置,本转移仓仅由仓体、仓盖及扭簧组成,部件结构简单、制备难度低,可有效降低制造成本,便于在各类实验室中推广使用,解决了现有真空转移装置难以普及的问题。其次,本发明的X射线光电子能谱样品转移仓操作简便,无需依赖操作人员的熟练程度,操作人员仅需拨动仓盖的盖体外露解锁部,即可使盖体插接部上的卡扣凸起与仓体开口内壁的卡扣凹槽脱离卡合,在扭簧的弹性力作用下,仓盖会自动朝外翻转脱离仓体并避让仓体的开口,操作步骤简单、便捷,解决了现有快速转移法对操作人员熟练度要求高、操作难度大的缺陷。还有,本发明的X射线光电子能谱样品转移仓可有效避免X射线光电子能谱样品在转移过程中接触空气,仓体的容置腔可稳定容置XPS样品,盖体插接部插入容置腔后,盖体外露解锁部能紧密覆盖仓体的开口,且卡扣凸起与卡扣凹槽的卡合结构可确保仓体与仓盖的连接密封性,配合扭簧的弹性复位作用,无论是样品放入容置腔后的密封保存,还是转移至XPS仪器时的开盖操作,均能最大限度隔绝空气,避免空气敏感型样品发生氧化、水解等反应,保障XPS分析数据的准确性与可靠性,解决了现有快速转移法无法完全避免空气暴露、数据重复性差的问题。

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Abstract

This invention provides an X-ray photoelectron spectroscopy (XPS) sample transfer chamber and its transfer method. The XPS sample transfer chamber includes a chamber body, a chamber cover, and a torsion spring. The chamber body has a receiving cavity for accommodating XPS samples, and the chamber body has an opening communicating with the receiving cavity. The inner wall of the opening has a snap-fit ​​groove. The chamber cover includes a cover insertion part and a cover external unlocking part connected to the cover insertion part. The end of the cover insertion part near the cover external unlocking part has a snap-fit ​​protrusion. The cover insertion part passes through the opening and is inserted into the receiving cavity. The cover external unlocking part tightly covers the opening, and the snap-fit ​​protrusion engages with the snap-fit ​​groove. One end of the torsion spring is connected to the chamber body, and the other end of the torsion spring is connected to the chamber cover. The torsion spring has an elastic force for driving the chamber cover to flip outward. By moving the cover external unlocking part, the snap-fit ​​protrusion disengages from the snap-fit ​​groove, thereby causing the chamber cover to flip outward under the elastic force of the torsion spring, detaching from the chamber body and avoiding the opening.
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Description

Technical Field

[0001] This invention relates to the field of X-ray photoelectron spectroscopy, and more particularly to an X-ray photoelectron spectroscopy sample transfer chamber and its transfer method. Background Technology

[0002] X-ray photoelectron spectroscopy (XPS) is a surface-sensitive analytical technique whose core function is to accurately determine the elemental composition and chemical state of a material's surface. It has irreplaceable application value in materials science, energy, and related research fields. In actual experimental research, many materials to be analyzed (such as lithium metal anodes and sulfide solid electrolytes) exhibit extremely high air sensitivity. Once these materials come into contact with air, they are highly susceptible to oxidation, hydrolysis, and other chemical reactions, leading to changes in the material's surface state and ultimately affecting the accuracy and reliability of XPS analysis results.

[0003] Since the preparation of air-sensitive materials usually needs to be completed in an air-isolated environment such as an inert atmosphere glove box, and the testing environment of the XPS instrument is different from the preparation environment, the sample transfer process from the material preparation environment to the XPS instrument must be strictly air-isolated. This is a key prerequisite for ensuring the validity of XPS analysis data.

[0004] Currently, two main solutions are used in laboratories for transferring XPS samples, but both have significant limitations. One solution uses commercially available vacuum transfer devices. For example, Chinese utility model patent CN210427411U discloses a transfer device for retrievable air-sensitive XPS samples, including a sample holder and a sample cover. The sample cover 2 is placed on the sample holder 1, with the circular groove at the bottom of the sample cover 2 engaging with the annular positioning boss 3. A fixing frame secures the sample cover 2 and the sample holder 1. The vacuum tube 5 is connected to the vacuum gas distribution system to evacuate the chamber inside the sample cover 2 to a vacuum state. Afterwards, the vacuum stopcock is closed, and the fixing frame is removed. The device is then sent into the sample introduction chamber of the photoelectron spectrometer. Although this type of device can achieve airless sample transfer, it has the disadvantages of complex structure and high manufacturing cost, making it difficult to use in various laboratories and limiting its application scope. Secondly, the rapid transfer method is adopted. This method relies on the operator's operating speed and attempts to reduce air exposure by shortening the transfer time. However, it cannot fundamentally avoid sample contact with air, and it requires a high level of operator proficiency, making it difficult to operate. At the same time, it is easy to cause poor repeatability of experimental data due to differences in operation, which cannot meet the needs of accurate analysis.

[0005] In summary, existing XPS sample transfer methods cannot simultaneously address cost, ease of operation, and air isolation. Therefore, it is necessary to provide at least one X-ray photoelectron spectroscopy (XPS) sample transfer chamber that is low-cost, easy to operate, and prevents XPS samples from coming into contact with air during transfer, as well as a transfer method using this XPS sample transfer chamber to transfer XPS samples. Summary of the Invention

[0006] The primary objective of this invention is to provide an X-ray photoelectron spectroscopy sample transfer chamber that is low in cost, easy to operate, and prevents X-ray photoelectron spectroscopy samples from coming into contact with air during the transfer process.

[0007] The second objective of this invention is to provide an X-ray photoelectron spectroscopy sample transfer method that uses a low-cost, easy-to-operate X-ray photoelectron spectroscopy sample transfer chamber that avoids the X-ray photoelectron spectroscopy sample from coming into contact with air during the transfer process.

[0008] To achieve the aforementioned first objective, the present invention provides an X-ray photoelectron spectroscopy sample transfer chamber, comprising a chamber body, a chamber cover, and a torsion spring. The chamber body has a receiving cavity for accommodating X-ray photoelectron spectroscopy samples, and one end of the chamber body has an opening communicating with the receiving cavity. The inner wall of the opening has a snap-fit ​​groove. The chamber cover includes a cover insertion portion and an exposed unlocking portion connected to the cover insertion portion. The area of ​​the exposed unlocking portion facing the cover insertion portion is larger than the area of ​​the cover insertion portion facing the exposed unlocking portion. The cover insertion portion is closer to the exposed unlocking portion. The lock has a latching protrusion at its end. The cover insert passes through the opening in a sealed manner and is inserted into the receiving cavity. The exposed unlocking part of the cover tightly covers the opening, and the latching protrusion engages with the latching groove. One end of the torsion spring is connected to the compartment body, and the other end of the torsion spring is connected to the compartment cover. The torsion spring has an elastic force for driving the compartment cover to flip outward. By moving the exposed unlocking part of the cover, the latching protrusion disengages from the latching groove, thereby causing the compartment cover to flip outward under the elastic force of the torsion spring, disengaging from the compartment body and avoiding the opening.

[0009] Compared with existing technologies, the X-ray photoelectron spectroscopy sample transfer chamber of this invention is inexpensive and easy to popularize. Compared with the complex and expensive commercial vacuum transfer devices in the prior art, this transfer chamber consists only of a chamber body, a chamber cover, and a torsion spring. The component structure is simple and easy to manufacture, which can effectively reduce manufacturing costs and facilitate its use in various laboratories, solving the problem of the difficulty in popularizing existing vacuum transfer devices. Secondly, the X-ray photoelectron spectroscopy sample transfer chamber of this invention is easy to operate and does not rely on the operator's skill level. The operator only needs to move the exposed unlocking part of the cover to disengage the buckle protrusion on the cover insertion part from the buckle groove on the inner wall of the chamber opening. Under the elastic force of the torsion spring, the cover will automatically flip outward to disengage from the chamber body and avoid the opening of the chamber body. The operation steps are simple and convenient, solving the defects of existing rapid transfer methods that require high operator skill and are difficult to operate. Furthermore, the X-ray photoelectron spectroscopy sample transfer chamber of this invention can effectively prevent X-ray photoelectron spectroscopy samples from coming into contact with air during the transfer process. The chamber's accommodating cavity can stably accommodate XPS samples. After the cover insertion part is inserted into the accommodating cavity, the exposed unlocking part of the cover can tightly cover the opening of the chamber. Moreover, the engaging structure of the buckle protrusion and buckle groove can ensure the sealing of the connection between the chamber and the cover. Combined with the elastic reset action of the torsion spring, whether it is the sealed preservation after the sample is placed in the accommodating cavity or the opening operation when transferring to the XPS instrument, air can be isolated to the maximum extent, avoiding oxidation, hydrolysis and other reactions of air-sensitive samples, ensuring the accuracy and reliability of XPS analysis data, and solving the problem that existing rapid transfer methods cannot completely avoid air exposure and have poor data repeatability.

[0010] Preferably, the compartment includes a compartment body portion and a compartment connecting seat portion, the receiving cavity is formed inside the compartment body portion, the opening is opened on one end of the compartment body portion, the compartment connecting seat portion protrudes from the outer side wall of the compartment body portion and is located near the opening, and one end of the torsion spring is connected to the compartment connecting seat portion. Preferably, the housing connecting seat is provided with a positioning groove, and one end of the torsion spring is inserted and positioned in the positioning groove. Preferably, the positioning groove includes a positioning straight groove and a positioning bent groove respectively disposed in the compartment connecting seat. One end of the positioning straight groove forms a slot on the end face of the compartment connecting seat. One end of the positioning bent groove is connected to the other end of the positioning straight groove, and the positioning bent groove is bent relative to the positioning straight groove. One end of the torsion spring is inserted and positioned in the positioning straight groove and the positioning bent groove. Preferably, there is a movable gap between the torsion spring and the positioning groove. Preferably, the main body of the silo has a tubular structure. Preferably, the opening is circular, and the cover insertion part and the exposed unlocking part of the cover are also circular. Preferably, the buckle groove is arranged on the inner wall of the opening along the circumferential direction of the inner wall of the opening, and the buckle protrusion is arranged on the cover insertion part along the circumferential direction of the cover insertion part. To achieve the second objective mentioned above, the present invention provides an X-ray photoelectron spectroscopy (XPS) sample transfer method using the aforementioned XPS sample transfer chamber, comprising the following steps: (1) placing the XPS sample transfer chamber in a glove box filled with argon gas, and moving the exposed unlocking part of the cover to disengage the buckle protrusion from the buckle groove, thereby causing the chamber cover to flip outward under the elastic force of the torsion spring, disengaging from the chamber body and avoiding the opening; (2) in the glove box, placing the XPS sample to be tested... After the sample is prepared on the sample stage, the sample stage is placed directly into the accommodating cavity of the chamber, and then the chamber cover is pressed and locked onto the chamber, so that the cover insertion part passes through the opening and is inserted into the accommodating cavity, the exposed unlocking part of the cover tightly covers the opening, the buckle protrusion engages with the buckle groove, the torsion spring is in the energy storage state, at this time, the accommodating cavity of the chamber is filled with argon gas and isolated from the outside atmosphere; (3) the X-ray photoelectron spectroscopy sample transfer chamber is taken out from the glove box and transferred to the sample preparation room.

[0011] Compared with existing technologies, the X-ray photoelectron spectroscopy sample transfer method of the present invention has low transfer cost and is easy to popularize. The X-ray photoelectron spectroscopy sample transfer method relies on the X-ray photoelectron spectroscopy sample transfer chamber composed of the chamber body, chamber cover and torsion spring. It does not require the use of complex and expensive commercial vacuum transfer devices. The transfer process does not require additional high equipment costs. Moreover, the transfer chamber is simple to prepare and the cost is controllable, which makes the transfer method applicable in various laboratories and solves the problem of high equipment cost and difficulty in popularization of existing vacuum transfer methods. Secondly, the X-ray photoelectron spectroscopy sample transfer method of the present invention is simple to operate and requires low operator proficiency. It does not rely on complex operating skills. The operator only needs to follow the standard steps, and in an argon-filled glove box, move the exposed unlocking part of the cover to disengage the buckle protrusion on the cover from the buckle groove on the inner wall of the compartment opening. The opening of the compartment can then be opened by the elastic force of the torsion spring. After the sample stage is placed, simply press the cover to lock it, so that the buckle protrusion and buckle groove re-engage and the exposed unlocking part of the cover tightly covers the opening. The entire operation process is simple and easy to understand, and the steps are clear. It solves the defects of the existing rapid transfer method, which requires a high level of operator proficiency, is difficult to operate, and is prone to operational errors. Furthermore, the X-ray photoelectron spectroscopy sample transfer method of the present invention first places the X-ray photoelectron spectroscopy sample transfer chamber in an argon-filled glove box to complete the opening, sample stage placement, and chamber lid locking operations, so that the chamber's accommodating cavity is filled with argon and completely isolated from the outside atmosphere; throughout the transfer process, the locking structure between the chamber and the chamber lid remains sealed, and the energy storage state of the torsion spring ensures the stability of the chamber lid locking, which can effectively prevent outside air from entering the accommodating cavity and contacting the sample, thus avoiding contact between the X-ray photoelectron spectroscopy sample and air during the transfer process, ensuring the accuracy and reliability of XPS analysis data.

[0012] Preferably, the procedure also includes step (4): evacuating the sample preparation chamber to the required vacuum level, and having the operator use a hand probe to pry open the exposed unlocking part of the chamber cover, causing the buckle protrusion to disengage from the buckle groove, thereby causing the chamber cover to flip outward and detach from the chamber body under the elastic force of the torsion spring. The operator then uses the probe to enter the chamber body and remove the sample stage, and finally sends the sample stage into the XPS analysis chamber for testing. Attached Figure Description Figure 1 This is a three-dimensional structural diagram of the X-ray photoelectron spectroscopy sample transfer chamber of the present invention.

[0013] Figure 2 This is a front view of the X-ray photoelectron spectroscopy sample transfer chamber of the present invention.

[0014] Figure 3 This is a cross-sectional view of the X-ray photoelectron spectroscopy sample transfer chamber of the present invention.

[0015] Figure 4 yes Figure 3 Enlarged view of point A in the middle.

[0016] Figure 5 This is a structural diagram of the X-ray photoelectron spectroscopy sample transfer chamber of the present invention when the chamber cover is opened. Detailed Implementation

[0017] To illustrate the technical content, structural features, objectives, and effects of the present invention in detail, the following description is provided in conjunction with the embodiments and accompanying drawings.

[0018] Please see Figures 1 to 5 This invention provides an X-ray photoelectron spectroscopy sample transfer chamber 100, comprising a chamber body 1, a chamber cover 2, and a torsion spring 3. The chamber body 1 has a receiving cavity 11 for accommodating an X-ray photoelectron spectroscopy sample 201, and one end of the chamber body 1 has an opening 12 communicating with the receiving cavity 11. The inner wall of the opening 12 has a snap-fit ​​groove 121. The chamber cover 2 includes a cover insertion portion 21 and a cover exposed unlocking portion 22 connected to the cover insertion portion 21. The area of ​​the cover exposed unlocking portion 22 facing the cover insertion portion 21 is larger than the area of ​​the cover insertion portion 21 facing the cover exposed unlocking portion 22. The cover insertion portion 21 is close to the cover body. The exposed unlocking part 22 has a latching protrusion 211 at its end. The cover insertion part 21 passes through the opening 12 in a sealed manner and is inserted into the receiving cavity 11. The exposed unlocking part 22 tightly covers the opening 12, and the latching protrusion 211 engages with the latching groove 121. One end of the torsion spring 3 is connected to the chamber body 1, and the other end of the torsion spring 3 is connected to the chamber cover 2. The torsion spring 3 has an elastic force to drive the chamber cover 2 to flip outward. By moving the exposed unlocking part 22, the latching protrusion 211 disengages from the latching groove 121, thereby causing the chamber cover 2 to flip outward under the elastic force of the torsion spring 3, detach from the chamber body 1, and avoid the opening 12. The above structure, through the coordinated cooperation of the chamber body 1, the chamber cover 2, and the torsion spring 3, achieves both sealed storage of the sample and easy opening through a simple moving operation, taking into account both sealing performance and ease of operation. At the same time, the overall structure is simple, effectively controlling manufacturing costs. The flipping angle of the cover 2 can be 90 degrees, 100 degrees, 120 degrees or 180 degrees, etc., which can be determined by those skilled in the art according to actual needs.

[0019] Please see Figures 1 to 4In one embodiment, the compartment 1 includes a compartment body 13 and a compartment connecting seat 14. A receiving cavity 11 is formed within the compartment body 13, and an opening 12 is formed at one end of the compartment body 13. The compartment connecting seat 14 protrudes from the outer wall of the compartment body 13 and is located near the opening 12. One end of the torsion spring 3 is connected to the compartment connecting seat 14. The compartment connecting seat 14 provides a stable connection support point for the torsion spring 3, ensuring that the torsion spring 3 can be accurately installed near the opening 12. This ensures that the elastic force of the torsion spring 3 on the compartment cover 2 is in a reasonable direction, thereby ensuring that the compartment cover 2 can be smoothly rotated. Simultaneously, it prevents the installation position of the torsion spring 3 from shifting, which could affect the overall sealing performance and operational stability of the structure.

[0020] Furthermore, in one embodiment, the housing connecting seat 14 is provided with a positioning groove 141, and one end of the torsion spring 3 is inserted and positioned in the positioning groove 141. By providing the positioning groove 141, one end of the torsion spring 3 is positioned while preventing the torsion spring 3 from disengaging.

[0021] Specifically, in one embodiment, the positioning groove 141 includes a positioning straight groove 141a and a positioning bent groove 141b respectively disposed in the compartment connecting seat 14. One end of the positioning straight groove 141a forms a groove 141a1 on the end face of the compartment connecting seat 14. One end of the positioning bent groove 141b is connected to the other end of the positioning straight groove 141a, and the positioning bent groove 141b is bent relative to the positioning straight groove 141a. One end of the torsion spring 3 is inserted and positioned in the positioning straight groove 141a and the positioning bent groove 141b. The positioning straight groove 141a facilitates quick insertion and installation of one end of the torsion spring 3, while the positioning bent groove 141b provides a limiting stop for the end of the torsion spring 3, further enhancing the stability of the torsion spring 3 installation and effectively preventing the torsion spring 3 from coming out of the positioning groove 141 during elastic expansion and contraction. Simultaneously, the bent structure adapts to the installation angle of the torsion spring 3, ensuring that the elastic force of the torsion spring 3 can be accurately applied to the cover 2, guaranteeing the smoothness of the cover 2's flipping action. The shape and structure of the positioning groove 141 can be determined according to actual conditions and is not limited to the structure of this embodiment. Those skilled in the art can design the structure of the positioning groove 141 according to actual conditions, ensuring both the insertion and positioning of the torsion spring 3 and preventing it from coming out. The positioning groove 141 can precisely limit one end of the torsion spring 3, preventing the torsion spring 3 from shifting or falling off during long-term use or under stress, ensuring that the torsion spring 3 always maintains a stable connection state, ensuring the smoothness and reliability of the opening and closing action of the X-ray photoelectron spectroscopy sample transfer chamber 100, and extending the service life of the X-ray photoelectron spectroscopy sample transfer chamber 100.

[0022] Specifically, in one embodiment, there is a movable gap between the torsion spring 3 and the positioning groove 141. The movable gap provides room for the elastic deformation of the torsion spring 3, especially when the exposed unlocking part 22 of the cover is moved to disengage the buckle protrusion 211 from the buckle groove 121. However, this is not a limitation.

[0023] Please see Figure 1 In one embodiment, the main body 13 of the chamber is tubular. The tubular structure of the main body 13 is easy to process and manufacture, which can effectively reduce the preparation cost. At the same time, the inner wall of the tubular structure is smooth, which facilitates the insertion and removal of the sample stage 200. It can also make the internal space of the accommodating cavity 11 uniform, ensuring that argon gas can fully fill the accommodating cavity 11, achieving complete air isolation protection for the sample. In addition, the tubular structure has high strength, which can effectively protect the internal sample from external pressure damage.

[0024] Specifically, in one embodiment, the chamber cover 2 is provided with a slot for positioning the other end of the torsion spring 3, and the other end of the torsion spring 3 is inserted and positioned in the slot. By providing the slot, the other end of the torsion spring 3 is positioned while preventing the torsion spring 3 from detaching. The shape and structure of the slot can be determined according to the actual situation. Those skilled in the art can design the structure of the slot according to the actual situation to ensure that the torsion spring 3 can be inserted and positioned while preventing the torsion spring 3 from detaching. The slot and the positioning groove 141 of the chamber body connecting seat 14 cooperate with each other to achieve precise positioning of both ends of the torsion spring 3, ensuring that the installation angle and position of the torsion spring 3 are accurate, so that the torsion spring 3 can apply a stable elastic force to the chamber cover 2, while effectively preventing the two ends of the torsion spring 3 from falling off, ensuring the stability and service life of the overall structure of the X-ray photoelectron spectroscopy sample transfer chamber 100.

[0025] Please see Figures 1 to 3 In one embodiment, the opening 12 is circular, as are the cover insertion portion 21 and the exposed unlocking portion 22. The circular opening 12, cover insertion portion 21, and exposed unlocking portion 22 facilitate manufacturing and allow for a better fit and seal between the cover insertion portion 21 and the opening 12, improving the sealing performance of the accommodating cavity 11 and effectively preventing the entry of outside air. Furthermore, the circular structure eliminates sharp edges, preventing operator injury during operation and enhancing operational safety. Additionally, the circular structure facilitates the rotation and manipulation of the cover 2, making the opening operation smoother.

[0026] Please see Figure 4 and Figure 5In one embodiment, the snap-fit ​​groove 121 is arranged on the inner wall of the opening 12 along the circumferential direction of the inner wall of the opening 12, and the snap-fit ​​protrusion 211 is arranged on the cover insertion portion 21 along the circumferential direction of the cover insertion portion 21. The circumferentially arranged snap-fit ​​groove 121 and snap-fit ​​protrusion 211 can realize the circumferential full engagement of the compartment 1 and the compartment cover 2, making the engagement structure more firm and stable, improving the sealing performance of the accommodating cavity 11, and effectively preventing outside air from entering the accommodating cavity 11 through the engagement gap.

[0027] The X-ray photoelectron spectroscopy sample transfer chamber 100 of this invention is low in cost and easy to popularize. Compared with the complex and expensive commercial vacuum transfer devices in the prior art, this transfer chamber consists only of a chamber body 1, a chamber cover 2, and a torsion spring 3. The component structure is simple and easy to manufacture, which can effectively reduce manufacturing costs and facilitate its use in various laboratories, solving the problem of the difficulty in popularizing existing vacuum transfer devices. Secondly, the X-ray photoelectron spectroscopy sample transfer chamber 100 of this invention is easy to operate and does not rely on the operator's skill level. The operator only needs to move the exposed unlocking part 22 of the cover 2 to disengage the buckle protrusion 211 on the cover insertion part 21 from the buckle groove 121 on the inner wall of the opening of the chamber body 1. Under the elastic force of the torsion spring 3, the cover 2 will automatically flip outward to disengage from the chamber body 1 and avoid the opening 12 of the chamber body 1. The operation steps are simple and convenient, solving the defects of existing rapid transfer methods that require high operator skill and are difficult to operate. Furthermore, the X-ray photoelectron spectroscopy sample transfer chamber 100 of the present invention can effectively prevent the X-ray photoelectron spectroscopy sample 201 from coming into contact with air during the transfer process. The accommodating cavity 11 of the chamber body 1 can stably accommodate the XPS sample. After the cover insertion part 21 is inserted into the accommodating cavity 11, the exposed unlocking part 22 of the cover can tightly cover the opening 12 of the chamber body 1. Moreover, the engaging structure of the buckle protrusion 211 and the buckle groove 121 can ensure the sealing of the connection between the chamber body 1 and the cover 2. With the elastic reset effect of the torsion spring 3, whether it is the sealed preservation after the sample is placed in the accommodating cavity 11 or the opening operation when transferring to the XPS instrument, air can be isolated to the maximum extent, avoiding oxidation, hydrolysis and other reactions of air-sensitive samples, ensuring the accuracy and reliability of XPS analysis data, and solving the problem that the existing rapid transfer method cannot completely avoid air exposure and has poor data repeatability.

[0028] Combination Figures 1 to 5 The present invention also provides an X-ray photoelectron spectroscopy sample transfer method using the X-ray photoelectron spectroscopy sample transfer chamber 100 of any of the above embodiments.

[0029] Example 1: The X-ray photoelectron spectroscopy sample transfer method includes the following steps: S11, place the X-ray photoelectron spectroscopy sample transfer chamber 100 in a glove box filled with sufficient argon gas, and move the exposed unlocking part 22 of the cover to disengage the buckle protrusion 211 from the buckle groove 121, so that the chamber cover 2 flips outward under the elastic force of the torsion spring 3 to detach from the chamber body 1 and avoid the opening 12. S12, In the glove box, after the X-ray photoelectron spectroscopy sample 201 to be tested is prepared on the sample stage 200, the sample stage 200 is placed directly into the accommodating cavity 11 of the chamber 1, and then the chamber cover 2 is pressed and locked onto the chamber 1, so that the cover insertion part 21 passes through the opening 12 and is inserted into the accommodating cavity 11, the exposed unlocking part 22 of the cover tightly covers the opening 12, the buckle protrusion 211 engages with the buckle groove 121, the torsion spring 3 is in the energy storage state, at this time, the accommodating cavity 11 of the chamber 1 is filled with argon gas and isolated from the outside atmosphere; S13, remove the X-ray photoelectron spectroscopy sample transfer chamber 100 from the glove box and transfer it to the sample preparation chamber.

[0030] Example 2: S21, place the X-ray photoelectron spectroscopy sample transfer chamber 100 in a glove box filled with sufficient argon gas, and move the exposed unlocking part 22 of the cover to disengage the buckle protrusion 211 from the buckle groove 121, so that the chamber cover 2 flips outward under the elastic force of the torsion spring 3 to detach from the chamber body 1 and avoid the opening 12. S22, In the glove box, after the X-ray photoelectron spectroscopy sample 201 to be tested is prepared on the sample stage 200, the sample stage 200 is placed directly into the accommodating cavity 11 of the chamber 1, and then the chamber cover 2 is pressed and locked onto the chamber 1, so that the cover insertion part 21 passes through the opening 12 and is inserted into the accommodating cavity 11, the exposed unlocking part 22 of the cover tightly covers the opening 12, the buckle protrusion 211 engages with the buckle groove 121, the chamber cover 2 and the chamber 1 remain closed and sealed, the torsion spring 3 is in the energy storage state, at this time, the accommodating cavity 11 of the chamber 1 is filled with argon gas and isolated from the outside atmosphere; S23, the X-ray photoelectron spectroscopy sample transfer chamber 100 is taken out of the glove box and transferred to the sample preparation chamber. Under the action of the locking protrusion 211 and the locking groove 121, the gas environment inside the chamber 1 is maintained throughout the transfer process, and the sample does not come into contact with the atmosphere. S24, evacuate the sample preparation chamber (or transition chamber) to the required vacuum level. The operator uses a handheld probe to pry open the exposed unlocking part 22 of the cover 2, causing the buckle protrusion 211 to disengage from the buckle groove 121. The moment the buckle protrusion 211 disengages from the buckle groove 121, the cover 2 loses its locking force, and the torsion spring 3 releases its elastic potential energy instantly. As a result, the cover 2 flips outward and detaches from the chamber 1 under the elastic force of the torsion spring 3. The cover 2 is pushed open to a position that completely avoids the opening 12 of the chamber 1. The top of the opening of the chamber 1 is completely open without any obstruction, allowing the probe to enter the receiving cavity 11 of the chamber 1 straight up and down without any obstruction to take samples. The operator then uses the probe to enter the interior of the chamber 1 and remove the sample stage 200. Finally, the sample stage 200 is sent into the XPS analysis chamber for testing.

[0031] The X-ray photoelectron spectroscopy sample transfer method of the present invention is low in cost and easy to popularize. The X-ray photoelectron spectroscopy sample transfer method relies on the X-ray photoelectron spectroscopy sample transfer chamber 100 composed of the chamber body 1, chamber cover 2 and torsion spring 3. It does not require the use of complex and expensive commercial vacuum transfer devices. The transfer process does not require additional high equipment costs. Moreover, the preparation of the transfer chamber is simple and the cost is controllable, which makes the transfer method applicable to various laboratories and solves the problem of high equipment cost and difficulty in popularization of existing vacuum transfer methods. Secondly, the X-ray photoelectron spectroscopy sample transfer method of the present invention is simple to operate and requires low operator proficiency. It does not rely on complex operating skills. The operator only needs to follow the standard steps and move the exposed unlocking part 22 of the cover 2 in an argon-filled glove box to disengage the buckle protrusion 211 on the cover insertion part 21 from the buckle groove 121 on the inner wall of the opening of the chamber 1. The opening 12 of the chamber 1 can be opened with the help of the elastic force of the torsion spring 3. After the sample stage 200 is placed, the cover 2 can be locked by pressing it, so that the buckle protrusion 211 and the buckle groove 121 re-engage and the exposed unlocking part 22 of the cover tightly covers the opening 12. The entire operation process is simple and easy to understand, and the steps are clear. It solves the defects of the existing rapid transfer method, which requires a high level of operator proficiency, is difficult to operate, and is prone to operation errors. Furthermore, the X-ray photoelectron spectroscopy sample transfer method of the present invention first places the X-ray photoelectron spectroscopy sample transfer chamber 100 in an argon-filled glove box to complete the opening, sample stage 200 placement, and chamber cover 2 locking operations, so that the accommodating cavity 11 of the chamber body 1 is filled with argon and completely isolated from the outside atmosphere; throughout the transfer process, the locking structure of the chamber body 1 and the chamber cover 2 remains sealed, and the energy storage state of the torsion spring 3 ensures the stability of the chamber cover 2 locking, which can effectively prevent outside air from entering the accommodating cavity 11 and contacting the sample, and can avoid the X-ray photoelectron spectroscopy sample 201 from contacting air during the transfer process, thus ensuring the accuracy and reliability of XPS analysis data.

[0032] The above-disclosed embodiments are merely preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. Therefore, any equivalent variations made in accordance with the claims of the present invention are still within the scope of the present invention.

Claims

1. An X-ray photoelectron spectroscopy sample transfer pod, characterized by, include: The chamber has a cavity for accommodating X-ray photoelectron spectroscopy samples, and one end of the chamber has an opening communicating with the cavity. The inner wall of the opening has a snap-fit ​​groove. A storage lid, comprising a lid insert portion and an exposed unlocking portion connected to the lid insert portion, wherein the area of ​​the exposed unlocking portion facing the lid insert portion is larger than the area of ​​the lid insert portion facing the exposed unlocking portion, and a snap-fit ​​protrusion is provided on the end of the lid insert portion near the exposed unlocking portion, the lid insert portion passing through the opening in a sealing manner and being inserted into the receiving cavity, the exposed unlocking portion tightly covering the opening, and the snap-fit ​​protrusion engaging with the snap-fit ​​groove; A torsion spring, one end of which is connected to the compartment body and the other end of which is connected to the compartment cover, has an elastic force for driving the compartment cover to flip outward; by moving the exposed unlocking part of the cover, the buckle protrusion is disengaged from the buckle groove, thereby causing the compartment cover to flip outward and detach from the compartment body under the elastic force of the torsion spring and avoid the opening.

2. The X-ray photoelectron spectroscopy sample transfer chamber of claim 1, wherein, The container includes a container body and a container connecting seat. The accommodating cavity is formed inside the container body. The opening is opened on one end of the container body. The container connecting seat protrudes from the outer side wall of the container body and is located near the opening. One end of the torsion spring is connected to the container connecting seat.

3. The X-ray photoelectron spectroscopy sample transfer chamber of claim 2, wherein, The connecting seat of the compartment is provided with a positioning groove, and one end of the torsion spring is inserted and positioned in the positioning groove.

4. The X-ray photoelectron spectroscopy sample transfer chamber of claim 3, wherein, The positioning groove includes a positioning straight groove and a positioning bent groove respectively disposed in the compartment connecting seat. One end of the positioning straight groove forms a slot on the end face of the compartment connecting seat. One end of the positioning bent groove is connected to the other end of the positioning straight groove, and the positioning bent groove is bent relative to the positioning straight groove. One end of the torsion spring is inserted and positioned in the positioning straight groove and the positioning bent groove.

5. The X-ray photoelectron spectroscopy sample transfer chamber of claim 3, wherein, There is a movable gap between the torsion spring and the positioning groove.

6. The X-ray photoelectron spectroscopy sample transfer chamber of claim 2, wherein, The main body of the silo has a tubular structure.

7. The X-ray photoelectron spectroscopy sample transfer chamber of claim 1, wherein, The opening is circular, as are the cover insertion part and the exposed unlocking part of the cover.

8. The X-ray photoelectron spectroscopy sample transfer chamber of claim 1, wherein, The buckle groove is arranged on the inner wall of the opening along the circumferential direction of the inner wall of the opening, and the buckle protrusion is arranged on the cover insertion part along the circumferential direction of the cover insertion part.

9. An X-ray photoelectron spectroscopy sample transfer method using the X-ray photoelectron spectroscopy sample transfer chamber as described in any one of claims 1-8, characterized in that, Includes the following steps: (1) Place the X-ray photoelectron spectroscopy sample transfer chamber in a glove box filled with argon gas, and move the exposed unlocking part of the cover to disengage the buckle protrusion from the buckle groove, so that the chamber cover flips outward under the elastic force of the torsion spring, disengages from the chamber body, and avoids the opening. (2) In the glove box, after the X-ray photoelectron spectroscopy sample to be tested is prepared on the sample stage, the sample stage is placed directly in the accommodating cavity of the chamber body, and then the chamber cover is pressed and locked on the chamber body, so that the cover insertion part passes through the opening and is inserted into the accommodating cavity, the exposed unlocking part of the cover body tightly covers the opening, the buckle protrusion engages with the buckle groove, the torsion spring is in the energy storage state, at this time, the accommodating cavity of the chamber body is filled with argon gas and isolated from the outside atmosphere; (3) Take the X-ray photoelectron spectroscopy sample transfer chamber out of the glove box and transfer it to the sample preparation chamber.

10. The X-ray photoelectron spectroscopy sample transfer method of claim 9, wherein, The procedure also includes step (4), whereby the sample preparation chamber is evacuated to the required vacuum level, and the operator uses a handheld probe to pry open the exposed unlocking part of the chamber cover, causing the buckle protrusion to disengage from the buckle groove, thereby causing the chamber cover to flip outward and detach from the chamber body under the elastic force of the torsion spring. The operator then uses the probe to enter the chamber body and remove the sample stage, and finally sends the sample stage into the XPS analysis chamber for testing.

Citation Information

Patent Citations

  • Transfer device for XPS recyclable air sensitive sample

    CN210427411U