Direct flight type three-dimensional atom probe ultra-high vacuum system and sample feeding method thereof

Abstract

The application discloses a direct flight type three-dimensional atom probe ultra-high vacuum system and a sample feeding method thereof. The ultra-high vacuum system comprises a sample feeding chamber, a transition chamber and an analysis chamber, and the sample feeding chamber, the transition chamber and the analysis chamber are respectively connected with a first vacuum pumping unit, a second vacuum pumping unit and a third vacuum pumping unit. A first vacuum magnetic force rod and a sample stage capable of being lifted are horizontally arranged in the sample feeding chamber, and the first vacuum magnetic force rod is used for pushing the sample stage into the transition chamber. A second vacuum magnetic force rod is horizontally arranged in the transition chamber and used for pushing the sample stage into the analysis chamber, and the vertical position of the second vacuum magnetic force rod is aligned with the center of a local electrode area of the analysis chamber. A delay line detector is arranged in the analysis chamber, and the delay line detector is used for completing mass-to-charge ratio detection of ions obtained through field evaporation effect of sample surface atoms. Through the system, the sample needle tip can be directly aligned with the center of the local electrode area.

Description

Technical Field

[0001] This application belongs to the field of three-dimensional atomic probe technology, and particularly relates to a direct-flying three-dimensional atomic probe ultra-high vacuum system and its sample introduction method. Background Technology

[0002] Atomic probe tomography (APT) can map the three-dimensional composition of materials with sub-nanometer spatial resolution and, theoretically, has no detection limit on elemental mass. This technology possesses excellent mass spectrometry resolution, capable of distinguishing isotopes of different elements. Using the compositional information obtained from APT, it is possible to reveal how the distribution of specific elements affects material properties, thereby guiding the development of new materials or more accurately predicting the failure risk of materials during their service life. This technology can also be used to trace the history of the material itself or the geological region where it originated. Whether man-made materials (such as engineering alloys and semiconductor devices) or natural materials (such as minerals), their bulk typically possesses a complex multi-scale hierarchical structure. For crystalline materials, atoms are arranged in a lattice, which may contain solute atom substitution, interstitial atom filling, and various defects (such as vacancies, dislocations, and grain boundaries), as well as second phases, phase boundaries, or pores. Interactions also occur at the material-environment interface, leading to changes in composition and microstructure (such as oxidation and cracking). Furthermore, materials may also be amorphous or be artificial devices with a defined layered structure (such as thin films).

[0003] To achieve atomic-level compositional analysis, the core analytical chamber of APT must maintain an ultra-high vacuum environment exceeding 1 × 10⁻⁸ Pa. This extreme vacuum condition serves three key purposes: First, it ensures that ions evaporating from the sample surface do not collide with residual gas molecules on their path to the detector, thus guaranteeing the accuracy of time-of-flight mass spectrometry and the precision of atomic spatial positioning. Second, it minimizes the adsorption of residual hydrogen (H₂) molecules on the low-temperature sample tip within the vacuum chamber. These adsorbed hydrogen molecules, once ionized, generate strong interference signals, severely hindering the detection and analysis of actual hydrogen in the material. Furthermore, the ultra-high vacuum prevents residual reactive gas molecules (such as oxygen) from causing oxidation or arc breakdown of the sample tip, protecting the fragile nanoparticle-tip sample and ensuring successful data acquisition.

[0004] Currently, in existing three-dimensional atomic probe systems, samples are usually prepared as needle-tip samples. The center of the needle tip needs to be aligned with the center of the local electrode area to obtain better field evaporation effect. However, very precise positional calibration is required. Therefore, it is necessary to develop a three-dimensional atomic probe ultra-high vacuum system that can simplify the sample introduction process and accurately position the sample needle tip at the center of the local electrode. Summary of the Invention

[0005] The purpose of this application is to overcome the problems of the prior art by disclosing a direct-flying three-dimensional atomic probe ultra-high vacuum system and its sample introduction method, so as to obtain higher sample introduction efficiency and more reliable ultra-high vacuum system layout.

[0006] The objective of this application is achieved through the following technical solution: A direct-flying three-dimensional atomic probe ultra-high vacuum system, comprising: a sample delivery chamber, a transition chamber, and an analysis chamber. The sample delivery chamber, transition chamber, and analysis chamber are sequentially separated by an ultra-high vacuum isolation valve, and the sample delivery chamber, transition chamber, and analysis chamber are respectively connected to a first vacuum pumping unit, a second vacuum pumping unit, and a third vacuum pumping unit to complete the vacuum level configuration of each chamber. The sample delivery chamber is horizontally equipped with a first vacuum magnetic rod and a height-adjustable sample stage. The first vacuum magnetic rod is used to push the sample stage into the transition chamber. The transition chamber is horizontally equipped with a second vacuum magnetic rod, which is used to push the sample stage into the analysis chamber. The vertical position of the second vacuum magnetic rod is aligned with the center of the local electrode area of ​​the analysis chamber. The analysis chamber is equipped with a delay line detector, which is used to detect the mass-to-charge ratio of ions obtained by the field evaporation effect of atoms on the sample surface.

[0007] According to a preferred embodiment, the sample introduction process within the direct-flying three-dimensional atom probe ultra-high vacuum system includes: When the sample is on the sample stage, the lifting device at the bottom of the sample stage is adjusted so that the sample stage is directly aligned with the first vacuum magnetic rod, thereby aligning and connecting the first vacuum magnetic rod with the sample stage, transferring the sample stage to the transition chamber, and then disconnecting the connection between the first vacuum magnetic rod and the bottom of the sample stage, and closing the transition chamber. Adjust the lifting device at the bottom of the sample stage again. When the sample stage is raised again and aligned horizontally with the second vacuum magnetic rod, the second vacuum magnetic rod is aligned and connected with the sample stage, and then the sample stage is transferred to the analysis chamber. Since the second vacuum magnetic rod is fixed in the vertical position, the sample needle tip can be directly aligned with the center area of ​​the local electrode in the analysis chamber. After calibration, the second vacuum magnetic rod is disconnected from the sample stage and returns to the transition chamber. Finally, the isolation valve between the analysis chamber and the transition chamber is closed.

[0008] According to a preferred embodiment, the evacuation sequence of each chamber in the direct-flying three-dimensional atomic probe ultra-high vacuum system during sample introduction is as follows: Before the sample is placed into the sample delivery chamber, the sample delivery chamber, the transition chamber, and the analysis chamber achieve a vacuum level of 10⁻⁶ within each chamber based on the first vacuum pumping unit, the second vacuum pumping unit, and the third vacuum pumping unit, respectively. -7 Pa, 10 -8 Pa and 10 -9 Pa; After the sample is placed into the sample delivery chamber, the chamber is continuously evacuated until the vacuum level inside the chamber is restored to 10%. - 7 Pa, and after restoring the corresponding vacuum level, the sample stage is sent to the transition chamber; After the sample stage enters the transition chamber, the transition chamber is continuously evacuated until the vacuum level inside the chamber is restored to 10. -8 Pa, and after restoring the corresponding vacuum level, the sample stage is sent to the analysis chamber; After the sample stage enters the analysis chamber, the chamber is continuously evacuated until the vacuum level inside the chamber is restored to 10. -9 Pa, and after the corresponding vacuum level is restored, the delay line detector performs subsequent analysis and measurement.

[0009] According to a preferred embodiment, a first ultra-high vacuum isolation valve is provided between the analysis chamber and the transition chamber, and the first ultra-high vacuum isolation valve has an air-locking device. In ultra-vacuum mode, when the vacuum level of the analysis chamber is below 1×10⁻⁶ -8 When the pressure reaches 100 Pa, the first ultra-high vacuum isolation valve triggers the gas-locking device to protect the vacuum environment of the analysis chamber.

[0010] According to a preferred embodiment, the third vacuum pumping unit includes: a titanium sublimation composite ion pump, a third cold trap, and a third mechanical pump; The inlet of the titanium sublimation composite ion pump is connected to the analysis chamber via a third ultra-high vacuum valve, and the outlet of the titanium sublimation composite ion pump is connected to the third mechanical pump via a third cold trap and a third solenoid valve to perform vacuuming of the analysis chamber.

[0011] According to a preferred embodiment, the analysis chamber is further provided with an ultra-low temperature cooling device for controlling the temperature inside the analysis chamber, so that the analysis chamber can be in an ultra-low temperature state below 80 K.

[0012] According to a preferred embodiment, the analysis chamber is filled with an inert gas with a purity of 99.999%.

[0013] According to a preferred embodiment, the inert gas in the analysis chamber is one or a mixture of helium, neon, and argon.

[0014] According to a preferred embodiment, the first vacuum pumping unit includes: a first molecular pump, a first cold trap, and a first mechanical pump. The inlet of the first molecular pump is connected to the sample delivery chamber via a first ultra-high vacuum valve, and the outlet of the first molecular pump is connected to the first mechanical pump via the first cold trap and a first solenoid valve to perform vacuum pumping of the sample delivery chamber.

[0015] According to a preferred embodiment, the second vacuum pumping unit includes: a second molecular pump, a second cold trap, and a second mechanical pump. The inlet of the second molecular pump is connected to the transition chamber via a second ultra-high vacuum valve, and the outlet of the second molecular pump is connected to the second mechanical pump via the second cold trap and a second solenoid valve to perform vacuum pumping of the transition chamber.

[0016] The aforementioned main solution and its various further alternative solutions can be freely combined to form multiple solutions, all of which are solutions that can be adopted and are claimed in this application. Those skilled in the art, after understanding the solution of this application, will realize that there are many combinations based on the prior art and common general knowledge, all of which are technical solutions to be protected in this application, and will not be exhaustively listed here.

[0017] The beneficial effects of this application are: This direct-flying 3D atomic probe ultra-high vacuum system features a unique vacuum system layout. Based on the structure of a first vacuum magnetic rod, a sample stage, and a second vacuum magnetic rod, it achieves position adjustment during sample introduction. Furthermore, the vertical position of the second vacuum magnetic rod is aligned with the center of the local electrode area in the analysis chamber, allowing the sample tip to be directly aligned with the center of the local electrode area. This virtually eliminates the need for secondary position adjustment within the analysis chamber, effectively reducing the risk of sample drop and improving system reliability. Simultaneously, based on this structural design, the sample position adjustment process within the analysis chamber is simplified or eliminated, saving adjustment time and further improving sample introduction efficiency. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of the direct-flying three-dimensional atom probe ultra-high vacuum system of this application; Among them, 1-sample delivery chamber, 2-first vacuum magnetic rod, 3-sample stage, 4-first ultra-high vacuum valve, 5-first molecular pump, 6-first cold trap, 7-first solenoid valve, 8-first mechanical pump, 9-transition chamber, 10-second ultra-high vacuum valve, 11-second molecular pump, 12-second cold trap, 13-second solenoid valve, 14-second mechanical pump, 15-analysis chamber, 16-delay line detector, 17-first ultra-high vacuum isolation valve, 18-third ultra-high vacuum valve, 19-titanium sublimation composite ion pump, 20-third cold trap, 21-third solenoid valve, 22-third mechanical pump, 23-ultra-low temperature cooling device, 24-second ultra-high vacuum isolation valve, 25-second vacuum magnetic rod. Detailed Implementation

[0019] The following specific examples illustrate the implementation of this application. Those skilled in the art can easily understand other advantages and effects of this application from the content disclosed in this specification. This application can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of this application. It should be noted that, unless otherwise specified, the following embodiments and features in the embodiments can be combined with each other.

[0020] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0021] In the description of this application, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of this application is in use. They are only for the convenience of describing this application and simplifying the description, 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, and therefore should not be construed as a limitation on this application. In addition, the terms "first," "second," and "third," etc., are only used to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0022] Furthermore, terms such as "horizontal," "vertical," and "sag" do not imply that components must be absolutely horizontal or suspended, but rather that they can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal relative to "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0023] In the description of this application, it should also be noted that, unless otherwise expressly specified and limited, the terms "set up," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0024] Furthermore, it should be noted that unless otherwise specified in this application, the specific structures, connections, positions, power sources, etc. involved are all things that a person skilled in the art can know without creative effort based on the prior art.

[0025] Example 1 refer to Figure 1 As shown, this application discloses a direct-flying three-dimensional atomic probe ultra-high vacuum system, which includes a sample delivery chamber 1, a transition chamber 9, and an analysis chamber 15. The sample delivery chamber 1, the transition chamber 9, and the analysis chamber 15 are respectively connected to a first vacuum pumping unit, a second vacuum pumping unit, and a third vacuum pumping unit to complete the vacuum level configuration of each chamber.

[0026] Specifically, the first vacuum pumping unit includes a first molecular pump 5, a first cold trap 6, and a first mechanical pump 8. The inlet of the first molecular pump 5 is connected to the sample delivery chamber 1 via a first ultra-high vacuum valve 4, and the outlet of the first molecular pump 5 is connected to the first mechanical pump 8 via the first cold trap 6 and a first solenoid valve 7, so as to perform vacuum pumping of the sample delivery chamber 1.

[0027] The second vacuum pumping unit includes a second molecular pump 11, a second cold trap 12, and a second mechanical pump 14. The inlet of the second molecular pump 11 is connected to the transition chamber 9 via a second ultra-high vacuum valve 10, and the outlet of the second molecular pump 11 is connected to the second mechanical pump 14 via the second cold trap 12 and a second solenoid valve 13, so as to perform vacuum pumping of the transition chamber 9.

[0028] The third vacuum pumping unit includes a titanium sublimation composite ion pump 19, a third cold trap 20, and a third mechanical pump 22. The inlet of the titanium sublimation composite ion pump 19 is connected to the analysis chamber 15 via a third ultra-high vacuum valve 18, and the outlet of the titanium sublimation composite ion pump 19 is connected to the third mechanical pump 22 via the third cold trap 20 and a third solenoid valve 21 to perform vacuum pumping of the analysis chamber 15.

[0029] Preferably, the connecting pipe assembly within each vacuum unit is a seamless stainless steel corrugated pipe with a circular cross-section.

[0030] Preferably, the sample delivery chamber 1, the transition chamber 9, and the analysis chamber 15 are sequentially separated by a second ultra-high vacuum isolation valve 24 and a first ultra-high vacuum isolation valve 17. The second ultra-high vacuum isolation valve 24 functions to isolate the vacuum environment of the sample delivery chamber 1, thereby making the high vacuum environment of the transition chamber 9 independent. The first ultra-high vacuum isolation valve 17 functions to isolate the vacuum environment of the transition chamber 9, thereby making the ultra-high vacuum environment of the analysis chamber 15 independent.

[0031] Furthermore, the first ultra-high vacuum isolation valve 17 has an air-locking device, which, in ultra-high vacuum mode, when the vacuum level of the analysis chamber 15 is lower than 1×10⁻⁶, allows for air-locking. -8When the vacuum level in the analysis chamber 15 drops below 1 × 10⁻⁶ Pa, the first ultra-high vacuum isolation valve 17 triggers the gas-locking device to protect the vacuum environment. Specifically, the first ultra-high vacuum isolation valve 17 is a vacuum proportional valve with a back-locking function. Furthermore, the direct-flying three-dimensional atom probe ultra-high vacuum system is also equipped with an alarm device. When the vacuum level in the analysis chamber 15 is detected to be below 1 × 10⁻⁶ Pa, an alarm will be triggered. -7 It can issue an alarm immediately when Pa is reached.

[0032] Preferably, a first vacuum magnetic rod 2 and a height-adjustable sample stage 3 are horizontally arranged in the sample delivery chamber 1. The first vacuum magnetic rod 2 is used to push the sample stage into the transition chamber 9. A second vacuum magnetic rod 25 is horizontally arranged in the transition chamber 9 to push the sample stage into the analysis chamber 15, and the vertical position of the second vacuum magnetic rod 25 is aligned with the center of the local electrode area of ​​the analysis chamber 15. A delay line detector 16 is provided in the analysis chamber 15, and the delay line detector 16 is used to detect the mass-to-charge ratio of ions obtained by the field evaporation effect of atoms on the sample surface.

[0033] This direct-flying 3D atomic probe ultra-high vacuum system features a unique vacuum system layout. Based on the structure of a first vacuum magnetic rod, a sample stage, and a second vacuum magnetic rod, it achieves position adjustment during sample introduction. Furthermore, the vertical position of the second vacuum magnetic rod is aligned with the center of the local electrode area in the analysis chamber, allowing the sample tip to be directly aligned with the center of the local electrode area. This virtually eliminates the need for secondary position adjustment within the analysis chamber, effectively reducing the risk of sample drop and improving system reliability. Simultaneously, it simplifies or eliminates the sample position adjustment steps within the analysis chamber, saving adjustment time and further improving sample introduction efficiency.

[0034] Preferably, the sample delivery chamber 1, the transition chamber 9, and the analysis chamber 15 are cylindrical cavities made of stainless steel.

[0035] Preferably, the analysis chamber 15 is further equipped with an ultra-low temperature cooling device 23 to control the temperature within the analysis chamber 15, enabling the analysis chamber 15 to maintain an ultra-low temperature below 80 K. During sample analysis, the analysis chamber 15 is filled with helium, neon, or argon gas with a purity of 99.999%.

[0036] Example 2 Based on Example 1, this example discloses a sample introduction method for a direct-flying three-dimensional atom probe ultra-high vacuum system, the sample introduction method comprising: When the sample is on the sample stage 3, the sample stage is directly aligned with the first vacuum magnetic rod 2 by adjusting the lifting device at the bottom of the sample stage 3. Thus, the first vacuum magnetic rod 2 is aligned and connected with the sample stage 3, and the sample stage 3 is transferred to the transition chamber 9. Then, the connection between the first vacuum magnetic rod 2 and the bottom of the sample stage 3 is disconnected, and the transition chamber 9 is closed. The bottom lifting device of the sample stage 3 is adjusted again. When the sample stage 3 is raised again and aligned horizontally with the second vacuum magnetic rod 25, the second vacuum magnetic rod 25 is aligned and connected with the sample stage 3, and then the sample stage 3 is transferred to the analysis chamber 15. Since the second vacuum magnetic rod 25 is fixed in the vertical position, the sample needle tip can be directly aligned with the center area of ​​the local electrode in the analysis chamber 15. After calibration, the second vacuum magnetic rod 25 is disconnected from the sample stage 3 and returns to the transition chamber 9. Finally, the isolation valve between the analysis chamber 15 and the transition chamber 9 is closed.

[0037] This sample introduction method, based on the movement settings of the first vacuum magnetic rod 2, the sample stage 3, and the second vacuum magnetic rod 25, achieves position adjustment during the sample introduction process. Furthermore, the vertical position of the second vacuum magnetic rod 25 is aligned with the center of the local electrode area in the analysis chamber 15, allowing the sample tip to be directly aligned with the center of the local electrode area. This virtually eliminates the need for secondary position adjustment within the analysis chamber 15, effectively reducing the risk of sample drop and improving system reliability. Simultaneously, it simplifies or eliminates the sample position adjustment steps within the analysis chamber 15, saving adjustment time and further improving sample introduction efficiency.

[0038] Furthermore, the evacuation sequence of each chamber in the direct-flying three-dimensional atom probe ultra-high vacuum system during sample introduction can be as follows: Before the sample is placed into the sample delivery chamber 1, the sample delivery chamber 1, the transition chamber 9, and the analysis chamber 15 achieve a vacuum level of 10⁻⁶ within each chamber based on the first vacuum pumping unit, the second vacuum pumping unit, and the third vacuum pumping unit, respectively. -7 Pa, 10 -8 Pa and 10 -9 Pa.

[0039] After the sample is placed into sample delivery chamber 1, vacuum treatment is continuously performed on sample delivery chamber 1 until the vacuum level inside the chamber is restored to 10. -7 Pa, and after restoring the corresponding vacuum level, the sample stage 3 is sent to the transition chamber 9; After the sample stage 3 enters the transition chamber 9, the transition chamber 9 is continuously evacuated until the vacuum level inside the chamber is restored to 10. -8 Pa, and after restoring the corresponding vacuum level, the sample stage 3 is sent to the analysis chamber 15; After the sample stage 3 enters the analysis chamber 15, the analysis chamber 15 is continuously evacuated until the vacuum level inside the chamber is restored to 10%. -9 Pa, and after the corresponding vacuum level is restored, the delay line detector 16 performs subsequent analysis and measurement.

[0040] By setting differentiated vacuum levels for sample delivery chamber 1, transition chamber 9, and analysis chamber 15 in the system, the vacuum level of the corresponding chamber can be quickly adjusted after receiving the sample during the sample injection process, thereby improving the sample injection efficiency.

[0041] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. A direct-flying three-dimensional atomic probe ultra-high vacuum system, characterized in that, The direct-flying three-dimensional atomic probe ultra-high vacuum system includes: a sample delivery chamber (1), a transition chamber (9), and an analysis chamber (15). The sample delivery chamber (1), the transition chamber (9) and the analysis chamber (15) are sequentially separated by an ultra-high vacuum isolation valve, and the sample delivery chamber (1), the transition chamber (9) and the analysis chamber (15) are respectively connected to a first vacuum pumping unit, a second vacuum pumping unit and a third vacuum pumping unit to complete the vacuum configuration of each chamber; The sample delivery chamber (1) is horizontally equipped with a first vacuum magnetic rod (2) and a sample stage (3) that can be raised and lowered. The first vacuum magnetic rod (2) is used to push the sample stage (3) into the transition chamber (9). The transition chamber (9) is horizontally equipped with a second vacuum magnetic rod (25) for pushing the sample stage (3) into the analysis chamber (15). The vertical position of the second vacuum magnetic rod (25) is aligned with the center of the local electrode area of ​​the analysis chamber (15). The analysis chamber (15) is equipped with a delay line detector (16). The delay line detector (16) is used to detect the mass-to-charge ratio of ions obtained by the sample surface atoms through the field evaporation effect.

2. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 1, characterized in that, A first ultra-high vacuum isolation valve (17) is provided between the analysis chamber (15) and the transition chamber (9). The first ultra-high vacuum isolation valve (17) has an air-locking device. In ultra-vacuum mode, when the vacuum level of the analysis chamber (15) is lower than 1×10⁻⁶ -8 When Pa, the first ultra-high vacuum isolation valve (17) triggers the gas-locking device to protect the vacuum environment of the analysis chamber (15).

3. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 1, characterized in that, The analysis chamber (15) is also equipped with an ultra-low temperature cooling device (23) to complete the temperature control inside the analysis chamber (15) so that the analysis chamber (15) can be in an ultra-low temperature state below 80 K.

4. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 1, characterized in that, The analysis chamber (15) is filled with inert gas with a purity of 99.999%.

5. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 4, characterized in that, The inert gas in the analysis chamber (15) is one or more of helium, neon, and argon.

6. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 1, characterized in that, The first vacuum pumping unit includes a first molecular pump (5), a first cold trap (6), and a first mechanical pump (8). The inlet of the first molecular pump (5) is connected to the sample delivery chamber (1) via a first ultra-high vacuum valve (4), and the outlet of the first molecular pump (5) is connected to the first mechanical pump (8) via the first cold trap (6) and a first solenoid valve (7) to perform vacuum pumping of the sample delivery chamber (1).

7. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 1, characterized in that, The second vacuum pumping unit includes a second molecular pump (11), a second cold trap (12), and a second mechanical pump (14). The inlet of the second molecular pump (11) is connected to the transition chamber (9) via a second ultra-high vacuum valve (10), and the outlet of the second molecular pump (11) is connected to the second mechanical pump (14) via the second cold trap (12) and a second solenoid valve (13) to perform vacuum pumping of the transition chamber (9).

8. The direct-flying three-dimensional atom probe ultra-high vacuum system as described in claim 1, characterized in that, The third vacuum pumping unit includes: a titanium sublimation composite ion pump (19), a third cold trap (20), and a third mechanical pump (22). The inlet of the titanium sublimation composite ion pump (19) is connected to the analysis chamber (15) via the third ultra-high vacuum valve (18), and the outlet of the titanium sublimation composite ion pump (19) is connected to the third mechanical pump (22) via the third cold trap (20) and the third solenoid valve (21) to perform vacuuming of the analysis chamber (15).

9. A sample introduction method for a direct-flying three-dimensional atomic probe ultra-high vacuum system as described in any one of claims 1 to 8, characterized in that, The injection method includes: When the sample is on the sample stage (3), the sample stage (3) is directly aligned with the first vacuum magnetic rod (2) by adjusting the lifting device at the bottom of the sample stage (3), so that the first vacuum magnetic rod (2) is aligned and connected with the sample stage (3), and the sample stage (3) is transferred to the transition chamber (9). Then the connection between the first vacuum magnetic rod (2) and the bottom of the sample stage (3) is disconnected, and the transition chamber (9) is closed. Adjust the bottom lifting device of the sample stage (3) again. When the sample stage (3) is raised again and aligned horizontally with the second vacuum magnetic rod (25), the second vacuum magnetic rod (25) is aligned and connected with the sample stage (3), and then the sample stage (3) is transferred to the analysis chamber (15). Since the second vacuum magnetic rod (25) is fixed in the vertical position, the sample needle tip can be directly aligned with the center area of ​​the local electrode in the analysis chamber (15). After calibration, the second vacuum magnetic rod (25) is disconnected from the sample stage (3) and returns to the transition chamber (9). Finally, the isolation valve between the analysis chamber (15) and the transition chamber (9) is closed.

10. The injection method as described in claim 9, characterized in that, The evacuation sequence of each chamber in the direct-flying three-dimensional atom probe ultra-high vacuum system during sample introduction is as follows: Before the sample is placed into the sample delivery chamber (1), the sample delivery chamber (1), the transition chamber (9), and the analysis chamber (15) achieve a vacuum level of 10 in the chambers based on the first vacuum pumping unit, the second vacuum pumping unit, and the third vacuum pumping unit, respectively. -7 Pa, 10 -8 Pa and 10 -9 Pa; After the sample is placed into the sample delivery chamber (1), the sample delivery chamber (1) is continuously evacuated until the vacuum level inside the chamber is restored to 10%. -7 Pa, and after restoring the corresponding vacuum level, the sample stage (3) is sent to the transition chamber (9); After the sample stage (3) enters the transition chamber (9), the transition chamber (9) is continuously evacuated until the vacuum level inside the chamber is restored to 10%. -8 Pa, and after restoring the corresponding vacuum level, the sample stage (3) is sent to the analysis chamber (15); After the sample stage (3) enters the analysis chamber (15), the analysis chamber (15) is continuously evacuated until the vacuum level inside the chamber is restored to 10%. -9 Pa, and after the corresponding vacuum level is restored, the delay line detector (16) performs subsequent analysis and measurement.

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