Ultrahigh vacuum transfer test device and method connected with test systems of different models

By designing an ultra-high vacuum transfer testing device including a vacuum cavity, a sample storage device and a transfer stub, the problem of bulkiness of the ultra-high vacuum transfer chamber and incompatible shape of the sample holder in the prior art is solved, and efficient and safe sample transfer and multiple characterization tests are achieved.

CN119827782APending Publication Date: 2025-04-15DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202311332960.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-13
Publication Date
2025-04-15

AI Technical Summary

Technical Problem

The existing ultra-high vacuum transfer chamber is bulky and different instrument manufacturers have inconsistent requirements for sample holder shape, resulting in low sample transfer efficiency and incompatibility.

Method used

An ultra-high vacuum transfer test device including a vacuum cavity, a sample storage device and a transit stake is designed. The vacuum cavity adopts a stainless steel cavity body, a plug valve, an ion pump and a window flange. The sample storage device is equipped with a magnetic rod, an adjustable angle short tube and a rotating linear drive. The transit holder can adapt to the shape of the sample slot of different instruments.

Benefits of technology

It realizes efficient ultra-high vacuum transfer of the same sample between different equipment, improves sample transfer efficiency, solves the problem of inconsistent requirements for sample holder shapes of different instrument manufacturers, and ensures the safety and integrity of the sample during the transfer process.

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Abstract

The invention provides an ultrahigh vacuum transfer test device and method connected with test systems of different models. The device comprises a vacuum cavity, a sample storage device and a transfer support, the vacuum cavity comprises a stainless steel cavity main body, a gate valve, an ion pump and a window flange, the gate valve is connected to the stainless steel cavity main body, is used for isolating an internal vacuum environment from an external atmospheric environment and is connected with a rapid sample introduction cavity, and the ion pump is connected with the stainless steel cavity main body and is used for isolating the internal vacuum environment from the external atmospheric environment. The vacuum chamber is used for maintaining internal vacuum, the window flange is used for observing internal conditions, the sample storage device is used for storing samples needing to be transferred and adjusting the spatial positions of the samples, and the transfer support is used for loading single-layer support samples. According to the invention, the same sample can be effectively subjected to various characterization tests through ultrahigh vacuum transfer, vacuum interconnection is realized, the sample transfer efficiency is effectively improved, the problem that different instrument manufacturers have different requirements on the shape of the sample support is solved, and the same sample can be subjected to various characterization tests in different equipment.
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Description

Technical Field

[0001] The present invention relates to the field of ultra-high vacuum transfer technology, and in particular to an ultra-high vacuum transfer test device and method for connecting different types of test systems. Background Art

[0002] There are various ultra-high vacuum characterization methods, including scanning tunneling microscopy (STM), X-ray photoelectron spectroscopy (XPS), high-resolution electron energy loss spectroscopy (HREELS), ion scattering spectroscopy (ISS), light emission electron microscopy (PEEM), low-energy electron diffraction (LEED) and ultraviolet photoelectron spectroscopy (UPS). Usually, researchers need to combine multiple characterization methods to have a deeper understanding of the surface structure and physical and chemical properties of samples. For example, STM can obtain the structural information of the atomic arrangement of the sample surface, XPS can obtain the valence information of the species on the sample surface, and HREELS can determine the information of the surface adsorbed species. Based on the combination of multiple characterization methods, the physical and chemical properties of the sample will have a deep and three-dimensional understanding. Therefore, it is necessary to characterize the same sample with multiple methods.

[0003] For ultra-high vacuum transfer technology, to ensure vacuum interconnection, the sample must first be in an ultra-high vacuum environment during the entire transfer process. This requires that the cavity for transferring the sample has a sufficiently good sealing performance and a good and portable exhaust pump or suction pump to maintain the vacuum, so as to ensure that the same sample does not change during the transfer process. On the other hand, it is required that the cavity connected to the transfer cavity can be emptied quickly and conveniently, thereby improving the efficiency of the entire transfer process. Therefore, a mature ultra-high vacuum transfer test device for connecting different types of test systems is required.

[0004] At present, different characterization tests need to be performed on the same sample. If the device itself is not integrated, it is necessary to conduct experiments on the device that integrates the characterization method. The common practice of each laboratory is to let the experimenter re-conduct the experiment on the corresponding equipment. However, for different equipment, the sample growth conditions are not the same, and the experimental process is inevitably different. Therefore, it is difficult to ensure that the experimental phenomenon is completely repeated, and the experimental process is inefficient. It takes a long time for the experimenter to adapt to the new equipment to conduct experiments. At present, there are also reports on related ultra-high vacuum suitcases on the market, but it needs to be directly connected to the main cavity to grab the sample for transfer, and the main cavity is generally not easy to emptied, because it needs to be baked at high temperature for a long time to restore the vacuum after emptying. And the overall is relatively bulky, there is no rotary linear drive installed, the sample rack height cannot be accurately controlled, and the sample rack has the risk of suddenly falling and damaging the sample. This type of suitcase is only suitable for occasional long-distance transportation of samples. At the same time, it does not involve transfer trays, and cannot overcome the problem of incompatibility between sample trays of different instruments and equipment. It is not suitable for transfer tests between multiple ultra-high vacuum equipment. Therefore, for laboratories conducting ultra-high vacuum experiments, a set of lightweight, mature and reliable ultra-high vacuum transfer test equipment is very necessary. Summary of the invention

[0005] In order to solve the current problem of bulky vacuum transfer chambers and the inconsistent requirements on sample holder shapes among different instrument manufacturers, the present invention provides a set of mature and efficient ultra-high vacuum transfer test devices, which can realize multiple characterization tests on different devices for the same sample after ultra-high vacuum transfer.

[0006] The technical means adopted by the present invention are as follows:

[0007] An ultra-high vacuum transfer test device connected to different types of test systems, comprising a vacuum chamber, a sample storage device and a transfer tray, wherein the vacuum chamber comprises a stainless steel chamber body, a gate valve, an ion pump and a window flange, wherein the gate valve is connected to the stainless steel chamber body and is used to isolate an internal vacuum environment from an external atmospheric environment and is connected to a fast sample injection chamber, wherein the ion pump is connected to the stainless steel chamber body and is used to maintain an internal vacuum, wherein the window flange is used to observe internal conditions, wherein the sample storage device is used to store samples to be transferred and to adjust the spatial position of the samples, and wherein the transfer tray is used to load single-layer tray samples;

[0008] The transfer tray comprises a main body, a fixing spring and a fixing nut. The fixing spring is used to fix the loaded single-layer tray sample, and the fixing nut is used to connect and fix the main body and the fixing spring.

[0009] Furthermore, the sample storage device includes a sample storage rack, a magnetic rod, an angle-adjustable short tube and a rotary linear drive. The sample storage rack is used to store samples that need to be transferred, the magnetic rod is used to control the up and down movement of the sample rack during sample transfer, the angle-adjustable short tube is used to adjust the angle of the magnetic rod, and the rotary linear drive is used to control the up and down movement of the magnetic rod during sample transfer.

[0010] Furthermore, the main body of the transfer tray is adapted to the shape of sample slots of different instruments.

[0011] The present invention also provides a method for using an ultra-high vacuum transfer test device connected to different types of test systems, comprising the following steps:

[0012] Step 1: Install the transfer chamber on the fast injection chamber through the gate valve, which is called the first fast injection chamber, turn off the ion pump, open the gate valve, and use a heating belt to bake the transfer chamber and the first fast injection chamber;

[0013] Step 2: After baking, start the ion pump while it is hot and close the gate valve;

[0014] Step 3, after the first rapid sample introduction cavity is cooled, the transfer tray is introduced into the main cavity through the first rapid sample introduction cavity;

[0015] Step 4: Grab the target single-layer tray through the swing rod and insert it into the transfer tray;

[0016] Step 5, grab the transfer tray loaded with the single-layer tray through the sample transfer rod of the first rapid sample injection chamber, and transfer it to the first rapid sample injection chamber;

[0017] Step 6, open the gate valve of the transfer chamber;

[0018] Step 7, adjusting the posture of the sample storage device, and lowering the sample storage rack to a suitable position to accommodate the sample transfer rod of the first rapid injection chamber;

[0019] Step 8: Insert the transfer tray into the sample slot of the sample storage rack, and then adjust the sample storage rack to rise to the highest position;

[0020] Step 9, close the gate valve of the transfer chamber to empty the first rapid injection chamber;

[0021] Step 10, removing the transfer chamber from the first rapid injection chamber;

[0022] Step 11, emptying the rapid sample injection chamber to be transferred into the device, which is called the second rapid sample injection chamber;

[0023] Step 12, installing the transfer chamber in the second rapid injection chamber through the plug valve, and then evacuating the second rapid injection chamber;

[0024] Step 13, after the second rapid sampling chamber is evacuated to an ideal vacuum, the transfer tray is transferred to the second rapid sampling chamber;

[0025] Step 14: close the gate valve of the transfer chamber, and transfer the transfer tray loaded with the single-layer tray sample into the corresponding chamber through the second rapid injection chamber for corresponding testing.

[0026] Furthermore, in step 1, the baking temperature is maintained at 100-150° C. for at least 48 hours.

[0027] Furthermore, during the transfer process, the transfer chamber maintains the power supply of the ion pump or converts the power supply of the ion pump into a mobile power supply based on the distance to be transferred.

[0028] Compared with the prior art, the present invention has the following advantages:

[0029] This equipment can effectively realize multiple characterization tests on the same sample through ultra-high vacuum transfer and realize vacuum interconnection. The transfer chamber is designed based on loadlock, which optimizes the transfer chamber structure and reduces its total mass. The magnetic rod is equipped with a rotary linear drive and the installation direction of the adjustable short tube is optimized to enable the sample storage rack to quickly adapt to the position of the sample transfer rod, effectively improving the sample transfer efficiency. The use of the transfer tray effectively solves the problem that different instrument manufacturers have different requirements for the shape of the sample tray, and realizes multiple characterization tests on the same sample in different equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0031] Figure 1 This is the front view of the transfer chamber structure of the present invention.

[0032] Figure 2 It is a side view of the transfer chamber structure of the present invention.

[0033] Figure 3 Schematic diagram of the sample storage rack of the present invention.

[0034] Figure 4 Schematic diagram of the transfer support in the present invention, wherein (a) is a front view; (b) is a side view; and (c) is a top view.

[0035] Figure 5 This is a schematic diagram of the transfer chamber of the present invention being installed on a loadlock.

[0036] Figure 6It is a schematic diagram of the transfer tray in the present invention.

[0037] Figure 7 This is a schematic diagram of the present invention using a wobble stick to load a single-layer tray on a transfer tray.

[0038] Figure 8 Schematic diagram of the transfer tray for loading a single-layer tray mounted on the Omicron multifunctional nanoprobe system. The single-layer tray sample comes from the NAP-STM system of SPECS.

[0039] Fig. 9 XPS spectra of the ZnO / Au(111) sample and the sample hydroxylated after high-pressure water treatment in the SPECS company's NAP-STM system and transferred to the Omicron multifunctional nanoprobe system via the ultra-high vacuum transfer device.

[0040] Fig.10 The sample holder used by NAP-STM developed by SPECS of Germany.

[0041] Fig.11 Sample holder for the Omicron multifunctional nanoprobe system.

[0042] Fig.12 The sample stage for the Omicron multifunctional nanoprobe system analysis chamber.

[0043] In the figure: 1: VAT gate valve; 2: stainless steel chamber body; 3: sample storage rack; 4: SAES NEXTorr Z100 ion pump; 5: window flange; 6: angle-adjustable short tube; 7: rotary linear drive clip; 8: magnetic rod; 9: rotary linear drive; 10: rotary linear drive threaded clip; 11: magnetic rod handle; 12: rotary linear drive clip; 13: rotary linear drive rotating handle; 14: wobble stick; 15: fixing nut; 16: single-layer sample holder; 17: fixing nut; 18: transfer holder body; 19: transfer holder fixing spring. DETAILED DESCRIPTION

[0044] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0045] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. The following description of at least one exemplary embodiment is actually only illustrative and is by no means intended to limit the present invention and its application or use. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0046] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit exemplary embodiments according to the present invention. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprising" and / or "including" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0047] Unless otherwise specifically stated, the relative arrangement of the parts and steps described in these embodiments, the numerical expressions and numerical values ​​do not limit the scope of the present invention. At the same time, it should be clear that, for ease of description, the sizes of the various parts shown in the drawings are not drawn according to the actual proportional relationship. The technology, methods and equipment known to ordinary technicians in the relevant field may not be discussed in detail, but in appropriate cases, the technology, methods and equipment should be regarded as part of the authorization specification. In all examples shown and discussed here, any specific value should be interpreted as merely exemplary, rather than as a limitation. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further discussed in subsequent drawings.

[0048] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by directional words such as "front, back, up, down, left, right", "lateral, vertical, perpendicular, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the drawings. They are only for the convenience of describing the present invention and simplifying the description. Unless otherwise specified, these directional words do not indicate or imply that the device or element referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of the present invention: the directional words "inside and outside" refer to the inside and outside relative to the contours of each component itself.

[0049] For ease of description, spatially relative terms such as "above", "above", "on the upper surface of", "above", etc. may be used here to describe the spatial positional relationship between a device or feature and other devices or features as shown in the figure. It should be understood that spatially relative terms are intended to include different orientations of the device in use or operation in addition to the orientation described in the figure. For example, if the device in the accompanying drawings is inverted, the device described as "above other devices or structures" or "above other devices or structures" will be positioned as "below other devices or structures" or "below their position devices or structures". Thus, the exemplary term "above" can include both "above" and "below". The device can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatially relative descriptions used here are interpreted accordingly.

[0050] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. If not otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the present invention.

[0051] like Figure 1 , Figure 2 As shown, the present invention provides an ultra-high vacuum transfer test device and method for connecting different types of test systems. The entire transfer chamber is designed based on the fast sample injection chamber (i.e., loadlock) equipped with each device. The fast sample injection chamber can be emptied at any time without destroying the vacuum of the main chamber, and a better vacuum can be quickly drawn after being emptied. As long as an ICF70 knife-edge flange is installed above the fast sample injection chamber, it can be connected to the transfer chamber, which greatly improves the sample transfer efficiency. Secondly, the sample transfer rod of the fast sample injection chamber is effectively used to grab the sample, which simplifies the transfer chamber structure and reduces the total mass. A rotary linear drive is installed on the magnetic rod of the transfer chamber, which can accurately control the height of the sample storage rack. The two screws on the left and right of the angle-adjustable short tube can effectively adjust the angle of the sample rack, so that the sample storage rack can quickly adapt to the sample transfer rod of the fast sample injection chamber, thereby improving the sample transfer efficiency. The transfer tray designed and produced can be designed with an upper single-layer tray into the sample tray shape required by commonly used equipment, and a lower one into the sample tray shape required by the equipment to be transferred. The single-layer tray is loaded on the transfer tray through the wobble stick (i.e., wobble stick) of commonly used equipment, and then the transfer tray loaded with the single-layer tray is transferred to other equipment through ultra-high vacuum for testing of other characterization methods.

[0052] Specifically, this embodiment discloses an ultra-high vacuum transfer test device for connecting different types of test systems, including a vacuum chamber, a sample storage device and a transfer tray. The vacuum chamber includes a stainless steel chamber body 2, a VAT gate valve 1, an ion pump 4 and a window flange 5. The stainless steel chamber body is used to connect various components and provide space. Specifically, the stainless steel chamber body is welded by a cylindrical chamber body and two cylindrical short tubes. The bottom is connected to the VAT gate valve 1 through an ICF70 knife-edge flange to isolate the atmosphere from the internal vacuum environment. The leakage rate is <1×10 -12 mbar / s. The left side is connected to the SAES NEXTorr Z100 ion pump 4 through the ICF70 knife-edge flange. The ion pump controller has an ion gauge that can read the vacuum value inside the chamber in real time. Through the exhaust of the SAES NEXTorr Z100 ion pump 4, the vacuum inside the transfer chamber can be achieved after high-temperature baking <2×10 -10 mbar. The right side is connected to the window flange 5 through the ICF70 knife-edge flange for observing the internal conditions of the chamber. The top is connected to the sample storage device through the ICF70 knife-edge flange.

[0053] The VAT plug valve is connected to the main body of the stainless steel cavity, which is used to isolate the internal vacuum environment from the external atmospheric environment and is connected to the fast sample injection cavity. The ion pump is connected to the main body of the stainless steel cavity to maintain the internal vacuum and read the internal vacuum. The window flange is used to observe the internal situation. The internal situation of the transfer cavity is observed through the window flange 5. When there is a risk of sample loss, the experiment is stopped urgently and the sample is taken out to prevent the sample from falling into the main device. The sample storage device is used to store the sample to be transferred and adjust the spatial position of the sample. The transfer tray is used to load the single-layer tray sample. The ultra-high vacuum transfer test device can realize the transfer of samples in different models of test systems based on the loadlock of each device. On the one hand, it can not destroy the ultra-high vacuum environment of the original cavity and realize rapid transfer. On the other hand, it can reduce the weight of the transfer cavity and reduce the total mass of the whole system to less than 10kg. Its matching transfer tray can perfectly solve the problem of incompatible sample tray shapes between different test instrument manufacturers, and realize the same sample on different instruments. Test. Therefore, this set of devices can realize sample transfer and testing in any ultra-high vacuum system and realize vacuum interconnection.

[0054] Furthermore, the sample storage device comprises: Figure 3The sample storage rack 3, magnetic rod, angle-adjustable short tube and rotary linear drive shown are used to store samples that need to be transferred. The sample storage rack 3 has a spring for clamping the stored samples to avoid the risk of sample loss during the sample transfer process. The magnetic rod is used to control the up and down movement of the sample rack during sample transfer, the angle-adjustable short tube is used to adjust the angle of the magnetic rod, and the rotary linear drive is used to control the up and down movement of the magnetic rod during sample transfer. By rotating the rotating handle 13, the rising or falling distance of the sample storage rack 3 can be accurately controlled. The left and right screws of the adjustable angle short tube 6 can quickly adjust the angle of the sample storage rack to adapt to the sample transfer rod of the fast sample injection chamber, which is convenient for grabbing samples. Specifically, the angle-adjustable short tube 6 is connected to the vacuum chamber body 2 and the magnetic rod 8 through an ICF70 knife-edge flange, wherein the rotary linear drive is fixed to the magnetic rod through two clips 7 and 12, and the handle 11 of the magnetic rod is fixed to another threaded clip 10 through a nut. The up and down movement of the sample storage rack can be completed by rotating the rotating handle 13.

[0055] As an optional embodiment, the angle-adjustable short tube 6 in the sample storage device is fixed with three studs, one of which is directed toward the direction of the gate valve handle. When the transfer chamber is installed, the gate valve handle is parallel to the loadlock sample transfer rod. By adjusting the other two studs of the angle-adjustable short tube 6, the angle of the sample storage rack 3 can be quickly matched with the loadlock sample transfer rod gripper.

[0056] More specifically, the sample storage device includes: a sample storage rack 3, an angle-adjustable short tube 6, a rotating linear drive clamp 7, a magnetic rod 8, a rotating linear drive 9, a rotating linear drive threaded clamp 10, a magnetic rod handle 11, a rotating linear drive clamp 12, and a rotating linear drive rotating handle 13. By rotating the rotating handle 13, the rising or falling distance of the sample storage rack 3 can be accurately controlled. By adjusting the left and right screws of the angle-adjustable short tube 6, the angle of the sample storage rack can be quickly adjusted to adapt to the sample transfer rod of the loadlock, thereby facilitating the grabbing of samples.

[0057] Furthermore, if Figure 4 , Figure 6As shown, the transfer tray includes: a fixing nut 15, a fixing nut 17, a transfer tray main body 18, a transfer tray fixing spring 19, the fixing spring is used to fix the loaded single-layer tray sample, and the fixing nut is used to connect the fixed main body and the fixing spring. Specifically, the two protruding cantilevers of the fixed spring 19 of the transfer tray are bent to a certain extent, so that the distance between the lowest position of the cantilever and the main body 18 is less than the thickness of the single-layer tray, so that the two cantilevers tightly press the single-layer tray to prevent the sample from falling during the sample transfer process. The transfer tray main body 18 can be designed into a sample tray shape required by an ultra-high vacuum system, and the thickness and other required shapes can be customized according to the equipment and experimental conditions. The loaded single-layer tray 16 can be designed into a sample tray shape required by another ultra-high vacuum system, so as to achieve equipment interconnection.

[0058] Furthermore, the main body of the transfer tray can adapt to the shape of sample slots of different instruments. Figure 7 As shown, the single-layer tray sample 16 is grabbed by the wobble stick 14 and inserted from right to left into the space between the fixed spring piece and the main part of the transfer tray.

[0059] The present invention also provides a method for using an ultra-high vacuum transfer test device that is connected to different types of test systems. The main steps are: loading the sample to be transferred and tested on a transfer tray and then transferring it into a transfer chamber, then removing the transfer chamber and installing it on the loadlock of a target device to be transferred into, and then transferring the loadlock of the target device to be transferred into the test chamber for testing after a better vacuum is drawn to the loadlock of the target device, thereby achieving ultra-high vacuum transfer testing of the same sample on different devices.

[0060] The specific steps include:

[0061] Step 1: Figure 5 As shown, the transfer chamber is installed on a loadlock of a common device, called loadlock-1, the SAES NEXTorr Z100 ion pump 4 is turned off, the VAT gate valve 1 is opened, and the transfer chamber and loadlock-1 are baked at 100-150°C using a heating tape for at least 48 hours.

[0062] Step 2: After stopping the baking, start the SAES NEXTorr Z100 ion pump 4 while it is still hot, and close the VAT gate valve 1.

[0063] Step 3: After loadlock-1 cools down, transfer the transfer tray into the main cavity through loadlock-1.

[0064] Step 4: Grab the target single-layer tray 16 with the wobble stick and insert it into the transfer tray from right to left.

[0065] Step 5: Grab the transfer tray loaded with the single-layer tray 16 through the sample transfer rod of loadlock-1 and transfer it to loadlock-1.

[0066] Step 6: Open the VAT gate valve 1 of the transfer chamber.

[0067] Step 7: Shake and rotate the handle 13 of the linear drive to lower the sample storage rack 3 to a suitable position to accommodate the loadlock-1 sample transfer rod.

[0068] Step 8: Adjust the left and right screws of the angle-adjustable short tube 6 to make the position of the sample storage rack 3 adapt to the loadlock-1 sample transfer rod.

[0069] Step 9: Insert the transfer tray into the sample slot of the sample storage rack 3, and shake the linear drive handle 13 to raise the sample storage rack 3 to the highest position.

[0070] Step 10: If long-distance transfer is required, the power supply of SAES NEXTorr Z100 ion pump 4 can be converted from AC power to 24V mobile power supply as quickly as possible. If short-distance transfer is required, the power cord can be connected and transferred together.

[0071] Step 11: Close the VAT gate valve 1 of the transfer chamber and vent loadlock-1.

[0072] Step 12. Remove the transfer chamber from loadlock-1.

[0073] Step 13: Empty the loadlock to be transferred to the device, called loadlock-2.

[0074] Step 14: Install loadlock-2 into the transfer chamber, tighten it, and then evacuate loadlock-2.

[0075] Step 15: After loadlock-2 reaches an ideal vacuum, repeat steps 3, 4, and 5.

[0076] Step 16: Use the sample transfer rod of loadlock-2 to grab the transfer tray and place it in loadlock-2, and shake the linear drive handle 13 to raise the sample storage rack 3 to the highest position.

[0077] Step 17: At this time, the SAES NEXTorr Z100 ion pump 4 is powered by a 24V mobile power supply, which is now switched to AC power supply and the mobile power supply is charged.

[0078] Step 18, close the VAT gate valve 1 of the transfer chamber, and transfer the transfer tray loaded with the single-layer tray sample into the corresponding chamber through loadlock-2 for corresponding testing.

[0079] Example 1

[0080] The laboratory has two sets of ultra-high vacuum experimental equipment. One set is NAP-STM developed by SPECS. The sample holder used is a standard rectangular shape, such as Fig.10 The other is the Omicron multifunctional nanoprobe system, which is equipped with XPS, ISS, UPS and other spectral characterization methods. The required sample holder shape and test chamber sample stage are as follows: Fig.11 and Fig.12 As shown, Fig.11 It can be seen that the sample holder shape required by Omicron is not only a rectangle, but also has two protruding "wings" near the ear of the sample holder. This is because the sample slot of the Omicron system is straight-through, and the sample needs the so-called "wings" to limit the position after being inserted into the sample slot to prevent the sample from being pushed through the sample slot. Fig.11 It can be seen that after the NAP-STM sample holder is loaded with a single crystal sample, if it is inserted into the Omicron analysis chamber sample stage, the detection surface is not the smooth surface of the single crystal sample, but the back surface. Therefore, the NAP-STM sample holder cannot be tested in the Omicron analysis chamber. In order to solve this problem, a transfer holder is designed. The lower part of the transfer holder is the sample holder with "wings" of the Omicron system. The upper part fixes a spring to the main part through a fixing nut. The two cantilevers extending from the spring are bent so that the distance between the lowest point of the cantilever and the main part is less than the thickness of the single-layer sample holder. Therefore, after the single-layer sample holder of the NAP-STM is grabbed by the wobble stick, the smooth surface of the single-layer holder sample is facing up and inserted into the transfer holder from right to left, ensuring that the transfer holder can detect the smooth surface of the single crystal after being inserted into the Omicron system analysis chamber sample stage. At the same time, because the cantilever exerts pressure on the single-layer holder, it effectively ensures that the single-layer holder does not fall during the transfer process. After that, the transfer tray loaded with the single-layer tray is transferred to the transfer chamber through the loadlock of the NAP-STM, and then the transfer chamber is removed and installed on the loadlock of the Omicron system. After the loadlock of the Omicron system is evacuated to a better vacuum, the sample can be transferred to the analysis chamber of the Omicron system through the loadlock of the Omicron system and the corresponding test can be carried out.

[0081] After application, the ZnO / Au(111) prepared by the NAP-STM system and the hydroxylated monolayer sample after high-pressure water treatment were first loaded on the transfer tray using this ultra-high vacuum transfer test device connected to different types of test systems. The transfer tray was then transferred to the Omicron multifunctional nanoprobe system through the transfer chamber to obtain the XPS spectra of the two samples. See Fig. 9After applying the present invention, the sample transfer efficiency is effectively improved. The use of the transfer tray effectively solves the problem that different instrument manufacturers have different requirements for the shape of the sample tray, and realizes multiple characterization tests on the same sample in different devices.

[0082] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An ultra-high vacuum transfer test device connected to different types of test systems, characterized in that: It includes a vacuum chamber, a sample storage device and a transfer tray, wherein the vacuum chamber includes a stainless steel chamber body, a gate valve, an ion pump and a window flange, wherein the gate valve is connected to the stainless steel chamber body and is used to isolate the internal vacuum environment from the external atmospheric environment and is connected to the fast injection chamber, wherein the ion pump is connected to the stainless steel chamber body and is used to maintain the internal vacuum, wherein the window flange is used to observe the internal situation, wherein the sample storage device is used to store the sample to be transferred and to adjust the spatial position of the sample, wherein the transfer tray is used to load the single-layer tray sample; The transfer tray comprises a main body, a fixing spring and a fixing nut. The fixing spring is used to fix the loaded single-layer tray sample, and the fixing nut is used to connect and fix the main body and the fixing spring.

2. The ultra-high vacuum transfer test device for connecting different types of test systems according to claim 1, characterized in that: The sample storage device includes a sample storage rack, a magnetic rod, an angle-adjustable short tube and a rotary linear drive. The sample storage rack is used to store samples that need to be transferred, the magnetic rod is used to control the up and down movement of the sample rack during sample transfer, the angle-adjustable short tube is used to adjust the angle of the magnetic rod, and the rotary linear drive is used to control the up and down movement of the magnetic rod during sample transfer.

3. The ultra-high vacuum transfer test device for connecting different types of test systems according to claim 1, characterized in that: The main body of the transfer tray is adapted to the shapes of sample slots of different instruments.

4. A method for using the ultra-high vacuum transfer test device for connecting different types of test systems according to any of claims 1 to 3, characterized in that: The steps include: Step 1: Install the transfer chamber on the fast injection chamber through the gate valve, which is called the first fast injection chamber, turn off the ion pump, open the gate valve, and use a heating belt to bake the transfer chamber and the first fast injection chamber; Step 2: After baking, start the ion pump while it is hot and close the gate valve; Step 3, after the first rapid sample introduction cavity is cooled, the transfer tray is introduced into the main cavity through the first rapid sample introduction cavity; Step 4: Grab the target single-layer tray through the swing rod and insert it into the transfer tray; Step 5, grab the transfer tray loaded with the single-layer tray through the sample transfer rod of the first rapid sample injection chamber, and transfer it to the first rapid sample injection chamber; Step 6, open the gate valve of the transfer chamber; Step 7, adjusting the posture of the sample storage device, and lowering the sample storage rack to a suitable position to accommodate the sample transfer rod of the first rapid injection chamber; Step 8: Insert the transfer tray into the sample slot of the sample storage rack, and then adjust the sample storage rack to rise to the highest position; Step 9, close the gate valve of the transfer chamber to empty the first rapid injection chamber; Step 10, removing the transfer chamber from the first rapid injection chamber; Step 11, emptying the rapid sample injection chamber to be transferred into the device, which is called the second rapid sample injection chamber; Step 12, installing the transfer chamber in the second rapid injection chamber through the plug valve, and then evacuating the second rapid injection chamber; Step 13: After the second rapid sample injection chamber is evacuated to an ideal vacuum, the transfer tray is transferred to the second rapid sample injection chamber; Step 14: close the gate valve of the transfer chamber, and transfer the transfer tray loaded with the single-layer tray sample into the corresponding chamber through the second rapid injection chamber for corresponding testing.

5. The method according to claim 4, characterized in that In step 1, the baking temperature is maintained at 100-150°C for at least 48 hours.

6. The method according to claim 4, characterized in that During the transfer process, the transfer chamber maintains the power supply of the ion pump or converts the power supply of the ion pump into a mobile power supply based on the distance to be transferred.