Vacuum spectroscopy test system

Abstract

The invention provides a vacuum spectroscopy testing system. The vacuum spectroscopy testing system comprises a supporting platform, a vacuum experiment cavity, a fluorescence detection system, a vacuum control system and a sample fine adjustment system installed above the vacuum experiment cavity. The sample fine adjustment system comprises a multi-sample bracket, a horizontal motor, a vertical motor and a rotating motor which are sequentially arranged from bottom to top; an anti-static wire is arranged between a metal sample frame of the multi-sample bracket and the second vacuum electric feed-through; a leading-out signal of the second vacuum electric feed-through is used as a TEY test signal; and a signal enhancement system is also arranged in the vacuum experiment cavity and comprises a bias ring fixed in the main body of the vacuum experiment cavity, a first vacuum electric feed-through electrically connected with the bias ring, and a positive voltage power supply connected with the first vacuum electric feed-through outside the cavity. According to the vacuum spectroscopy test system, the TEY test signal enhancement function is realized through the signal enhancement system, the signal-to-noise ratio of test data is improved, and the requirements of high-quality medium-energy XAS and high-energy TEY tests are met.

Description

Technical Field

[0001] The present invention belongs to the field of X-ray testing, and in particular relates to a vacuum spectroscopy testing system. Background Art

[0002] Synchrotron radiation medium-energy X-ray (2~5keV) technology can be used for K-edge XAS (X-ray absorption spectroscopy) testing of key elements such as P, S, Cl, K, Ca, V, and Ti. It is highly sensitive to the coordination field and valence state of 4d transition metals and plays a key role in environmental governance, agricultural ecology, biological and medical diagnosis, catalyst synthesis control, and dynamic process research of energy storage.

[0003] Intermediate-energy XAS is typically performed in an independent vacuum chamber. In practice, this requires frequent pumping and un-pumping of the chamber to change samples. This instantaneous pumping and un-pumping creates significant pressure differences within the chamber, which can damage thin Be windows and severely impact equipment in the optical path, including the accelerator. Therefore, a protective system must be designed for the intermediate-energy vacuum chamber to minimize damage to the optical path.

[0004] Synchrotron radiation total electron yield absorption spectroscopy (often abbreviated as TEY) has excellent surface sensitivity (typically a few nanometers) and spatial resolution, making it of great value in fields such as materials science, energy catalysis, and surface physics. TEY-mode XAS measurements typically require a vacuum chamber. The effective signal in TEY measurements is the Auger electrons generated by the sample's excitation. In practice, the TEY signal is not only accompanied by Auger electrons, but also contains a significant amount of unwanted secondary electrons and other background interference, resulting in a low signal-to-noise ratio. Therefore, the design of a medium-energy vacuum chamber must also consider the enhancement of the TEY signal in the high-energy region.

[0005] In summary, a medium-energy vacuum chamber must be equipped with a window protection system and a TEY signal enhancement system. However, the introduction of a window protection system will introduce various complex and difficult-to-remember operating procedures, prolong operation time, and fail to meet users' pursuit of convenient and efficient (fast) operation.

[0006] Therefore, there is an urgent need to design a vacuum spectroscopy testing system that can not only meet the needs of high-quality medium-energy XAS and high-energy TEY testing, but also save operation time and reduce possible misoperations to improve its user affinity. Summary of the Invention

[0007] The object of the present invention is to provide a vacuum spectroscopy test system to improve the signal-to-noise ratio of test data and meet the requirements of high-quality medium-energy XAS and high-energy TEY tests.

[0008] In order to achieve the above-mentioned objectives, the present invention provides a vacuum spectroscopy testing system, comprising a support platform, a vacuum experimental chamber and a fluorescence detection system, which are adjacent to each other and all installed on the support platform, a vacuum control system, and a sample fine-tuning system installed above the vacuum experimental chamber; the sample fine-tuning system comprises a multi-sample holder, a horizontal motor, a vertical motor and a rotary motor arranged in sequence from bottom to top; an anti-static wire is provided between the metal sample holder of the multi-sample holder and a second vacuum feedthrough; the lead-out signal of the second vacuum feedthrough serves as a TEY test signal; the vacuum experimental chamber is further provided with a signal enhancement system, the signal enhancement system comprising a bias ring fixed in the main body of the vacuum experimental chamber, a first vacuum feedthrough electrically connected to the bias ring, and a positive pressure power supply outside the chamber connected to the first vacuum feedthrough.

[0009] The main body of the vacuum test chamber is spherical, with an outer diameter of 300 mm and a wall thickness of 3 mm, and a plurality of flange interfaces are symmetrically distributed on the main body.

[0010] The vacuum test chamber satisfies at least one of the following:

[0011] a1) One of the flange interfaces is connected to the upstream X-ray optical path using a Be window;

[0012] a2) The outside of the vacuum test chamber is provided with an illumination lamp aligned with one of the flange interfaces and a camera aligned with one of the flange interfaces;

[0013] a3) one of the flange interfaces is provided with a first vacuum electrical feedthrough and one of the flange interfaces is provided with a second vacuum electrical feedthrough;

[0014] a4) A waste sample cleaning chamber is installed at the lower end of the vacuum test chamber. One end of the waste sample cleaning chamber is connected to a vacuum pump, and the other end is provided with a vacuum flange and a cleaning mask. A vacuum valve is installed between the vacuum test chamber and the waste sample cleaning chamber;

[0015] a5) A cylindrical tube is provided at the bottom of the vacuum test chamber. The cylindrical tube is provided with two thirteenth flange interfaces for connecting to the exhaust control system and four supporting feet. The fixing feet are used to fix the vacuum test chamber to the supporting platform.

[0016] The sample fine adjustment system further comprises a bellows which cooperates with the horizontal motor, the vertical motor and the rotary motor and is sealed with the vacuum experimental chamber.

[0017] The support platform includes an upper storage platform and a lower storage platform. The upper storage platform is an optical platform with M5 screw holes with a spacing of 5cm×5cm, which is used to fix the vacuum experimental chamber. The lower storage platform is a metal partition for placing and fixing related equipment and experimental instruments.

[0018] The support platform also includes an adapter plate, the vacuum test chamber is fixed on the adapter plate, and the adapter plate is fixed to the upper storage table by adapter plate fixing screws; four ejectors and four pressing plates are provided on the adapter plate, and the ejectors and pressing plates are both fixed on the upper storage table and are each provided with a horizontally retractable screw.

[0019] The fluorescence detection system includes a fluorescence detector, a motion motor arranged below the fluorescence detector, a detection system bellows connected between the fluorescence detector and the vacuum experimental chamber, and a motor bracket arranged between the motion motor and the support platform.

[0020] The vacuum control system includes a vacuum pump and multiple vacuum pipes connected between the vacuum experimental chamber and the vacuum pump; the multiple vacuum pipes are provided with electric valves with different pumping speeds, and all the electric valves are connected to a switch controller; the switch controller is configured to open and close different vacuum pipes to achieve slow pumping first and then fast pumping during pumping, thereby realizing the window protection function.

[0021] The bias ring is in the shape of a circular ring and is made of pure copper with an inner diameter of 50 mm, an outer diameter of 70 mm, and a thickness of 2 mm. The bias ring is fixed to the inner wall of the vacuum test chamber by three ceramic columns. The central axis of the bias ring is collinear with the central axis of the vacuum test chamber and is aligned with the multi-sample holder of the sample fine-tuning system. The distance from the center of the bias ring to the center of the sphere of the vacuum test chamber is 100 mm.

[0022] The multi-sample holder comprises a sample rod fixed on an eleventh flange interface on the top of the vacuum chamber, an insulating block mounted on the sample rod, a metal sample rack fixed by the insulating block, and a sample tray for mounting multiple samples.

[0023] The vacuum spectroscopy test system of the present invention realizes the TEY test signal enhancement function through the signal enhancement system. By applying an appropriate positive voltage on the bias ring, it can effectively reduce the coincidence or annihilation of low-kinetic energy Auger electrons on the sample surface, thereby increasing the effective signal ratio measured in the TEY test and improving the signal-to-noise ratio of the test data, meeting the needs of high-quality medium-energy XAS and high-energy TEY testing.

[0024] In addition, the present invention realizes slow vacuuming first and then rapid vacuuming through the vacuum control system during vacuuming, thereby realizing the window protection function, effectively reducing the impact of the pressure difference generated by the vacuum test chamber at the moment of vacuuming / breaking the vacuum on the thin Be window between the X-ray optical path and the vacuum test chamber, and at the same time, the vacuuming / breaking vacuum operation can be realized by one button of the switch controller, so that the vacuum test chamber can quickly reach the experimental state, reducing the complexity of operation while avoiding a series of serious consequences caused by misoperation. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1It is the overall structural diagram of the vacuum spectroscopy testing system of the present invention.

[0026] Figure 2 and Figure 3 It is an exploded view and an overall structural diagram of the vacuum spectroscopy test system of the present invention excluding the vacuum control system.

[0027] Figure 4 It is a structural diagram of the vacuum experimental chamber of the vacuum spectroscopy test system of the present invention.

[0028] Figure 5 and Figure 6 This is a diagram of the installation position of the waste sample cleaning chamber of the vacuum spectroscopy testing system of the present invention.

[0029] Figure 7 and Figure 8 This is a diagram showing the installation position of a sample fine adjustment system of the vacuum spectroscopy testing system of the present invention.

[0030] Figure 9 It is a structural diagram of the sample fine adjustment system of the vacuum spectroscopy testing system of the present invention.

[0031] Figure 10 It is a structural diagram of the support platform of the vacuum spectroscopy test system of the present invention.

[0032] Figure 11 It is an exploded diagram of the fluorescence detection system of the vacuum spectroscopy test system of the present invention.

[0033] Figure 12 It is an exploded view of the signal enhancement system and the multi-sample holder of the vacuum spectroscopy testing system of the present invention.

[0034] Figure 13 It is a cross-sectional view of the signal enhancement system and the multi-sample holder of the vacuum spectroscopy testing system of the present invention.

[0035] Figure 14 This is a schematic diagram of the structure of a typical flat-plate ionization chamber. DETAILED DESCRIPTION

[0036] The present invention will be further described below with reference to specific examples. It should be understood that the following examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0037] like Figure 1-Figure 3As shown, according to one embodiment of the present invention, the vacuum spectroscopy testing system of the present invention includes a vacuum chamber 100, a sample fine-tuning system 200, a fluorescence detection system 300, a vacuum control system 400, and a support platform 500. The vacuum chamber 100 and the fluorescence detection system 300 are adjacent to each other and are both mounted on the support platform 500. The vacuum control system 400 is also mounted on the support platform 500. The sample fine-tuning system 200 is mounted above the vacuum chamber 100.

[0038] The vacuum chamber 100 is removably mounted on the support platform 500, and its mounting position is adjustable, allowing for a wide range of coarse adjustments on the support platform 500 to align the vacuum chamber 100 with the experimental optical path. The sample fine-tuning system 200 is used to mount different samples for experiments and precisely adjust their positions. The fluorescence detection system 300 accurately adjusts the distance between the fluorescence detector and the sample for quantitative experiments.

[0039] like Figure 4 As shown, the vacuum chamber 100 adopts a spherical design with an outer diameter of 300 mm and a wall thickness of 3 mm. The dimensions of the vacuum chamber 100 can reduce the size of the experimental chamber to shorten the evacuation time while facilitating the precise installation of the external window during processing and the spatial layout of the external supporting systems during use. These external supporting systems specifically include: the incident X-ray pipeline, lighting, camera, fluorescence detection system 300 (opposite the sample inlet), transmission X-ray pipeline (opposite the incident X-ray pipeline), the extracavity motor (top) of the sample fine-tuning system 200, the exhaust port (bottom), the inlet pipeline interface, vacuum gauge / gauge, and the electronics system connected to the high vacuum electrical feedthrough.

[0040] like Figure 4 As shown, the main body of the vacuum chamber 100 is spherical, with multiple standard flange interfaces of different models (i.e., first flange interface 1 through eleventh flange interface 11) symmetrically distributed throughout the main body. The central axes of all flange interfaces pass through the center of the sphere. Except for interfaces with special purposes, the other interfaces (i.e., second flange interface 2, fourth flange interface 4, sixth flange interface 6, seventh flange interface 7, eighth flange interface 8, and ninth flange interface 9) are sealed with windows. The third flange interface 3 (i.e., the incident flange) must use a beryllium window, while the other interfaces can use windows. This design greatly enhances the internal lighting of the chamber, facilitating operator observation and adjustment of samples during experiments.

[0041] The central axes of the first flange interface 1, the second flange interface 2, the third flange interface 3, the fourth flange interface 4, the fifth flange interface 5, and the flange interfaces that are not marked due to obstruction and are directly opposite to the second flange interface 2, the third flange interface 3, and the fourth flange interface 4 are all on a horizontal plane passing through the center of the sphere, and the angle between the central axes of any two adjacent interfaces is 45°.

[0042] The first flange interface 1 , the second flange interface 2 , the third flange interface 3 , the fourth flange interface 4 , and the fifth flange interface 5 are all located on the same horizontal plane that runs through the vacuum test chamber 100 .

[0043] The first flange interface 1 is used to connect to the fluorescence detection system 300 . The size of the first flange interface 1 can accommodate the connection of most types of vacuum detector probes and leave room for adjustment.

[0044] The fifth flange interface 5 is used to secure a quick-open door with a rubber ring. The quick-open door has two functions: one is to allow sample replacement, and the other is to utilize the deformation principle of the rubber ring to ensure that when the quick-open door knob is loosened, the rubber ring gradually recovers, allowing gas exchange between the chamber and the outside world. This ensures that the air pressure in the chamber does not exceed 1 atmosphere, thereby protecting the thin Be window on the vacuum chamber 100. The inner diameter of the fifth flange interface 5 meets the requirements of single-handed sample replacement and nearby window installation.

[0045] The first flange interface 1 adopts the CF100 standard flange interface, the fifth flange interface 5 adopts the CF150 standard flange, the tenth flange interface 10 adopts the CF18 standard interface flange, and the eleventh flange interface 11 adopts the CF100 standard flange interface. Except for the first flange interface 1, the fifth flange interface 5, the tenth flange interface 10, and the eleventh flange interface 11 (i.e., the second flange interface 2 to the fourth flange interface 4, and the sixth flange interface 6 to the ninth flange interface 9), all flange interfaces other than the first flange interface 1, the fifth flange interface 5, the tenth flange interface 10, and the eleventh flange interface 11 (i.e., the second flange interface 2 to the fourth flange interface 4, and the sixth flange interface 6 to the ninth flange interface 9) are all CF35 standard flange interfaces.

[0046] The third flange interface 3 is sealed and connected to the upstream X-ray optical path using a Be window, serving as an incident flange. The flange interface (not shown) facing the third flange interface 3 is sealed and connected to the downstream, serving as an X-ray outlet.

[0047] The second flange interface 2 and the fourth flange interface 4 are sealed with windows and a camera aimed at the second flange interface 2 is provided outside the vacuum test chamber 100 . The camera is used to find and determine the position of the test sample in the chamber.

[0048] The sixth through ninth flange interfaces 6, 9 are located at a 45° angle directly above the horizontal plane that runs through the vacuum chamber 100. These interfaces are all sealed with sight windows. A lighting fixture is provided outside the sixth flange interface 6 to illuminate the chamber. The remaining windows serve as sight windows or other backup windows and can be easily replaced when needed.

[0049] The fourth flange interface 4 is sealed with a window and a lighting lamp is provided outside the vacuum chamber 100 and is aligned with the fourth flange interface 4. Thus, the sealing is achieved through the window, and the camera and the lighting lamp only need to be aligned to observe and illuminate through the window.

[0050] The tenth flange interface 10 is a standard interface flange of CF18, and a first vacuum electrical feedthrough with an SHV interface is installed on the flange for internal and external connections of the signal enhancement system.

[0051] The top of the vacuum chamber 100 is provided with an eleventh flange interface 11 for mounting the sample fine adjustment system 200 and a second vacuum electrical feedthrough with a BNC interface. The inner diameter of the eleventh flange interface 11 is sufficient to allow the sample stage to have a 5×5 cm range of motion in the horizontal plane.

[0052] A 20-cm-tall cylindrical tube 12 is installed at the bottom of the vacuum chamber 100. This tube 12 is equipped with two thirteenth flange interfaces 13 for connecting to the vacuum control system 200 and four support legs 14. The two thirteenth flange interfaces 13 are used to connect to the vacuum control system 200's slow inflation system and vacuum monitoring equipment, respectively. The fixing legs 14 secure the entire vacuum chamber 100 to the support platform 500. The thirteenth flange interface 13 uses a standard CF18 flange interface.

[0053] like Figure 5 and Figure 6 As shown, a waste sample cleaning chamber 101 is installed at the lower end of the vacuum chamber 100 (i.e., the bottom of the columnar tube 12). One end of the waste sample cleaning chamber 101 is connected to a waste sample cleaning vacuum pump, while the other end is equipped with a vacuum flange and a cleaning mask 103. Therefore, during experiments, when samples are mounted on a sample rack, there is always the possibility of accidental loss of samples and other debris. Such lost samples will remain in the waste sample cleaning chamber.

[0054] One end of the waste sample cleaning chamber 101 connected to the vacuum pump is equipped with a protective filter 102 to prevent waste samples from being sucked into the vacuum pump.

[0055] A vacuum valve 104 is installed between the vacuum chamber 100 and the waste sample cleaning chamber 101. To clean the waste sample, the vacuum valve is closed, the cleaning mask is opened, and the waste sample can be removed. This maintains the vacuum environment in the chamber, saving experimental time and preventing samples on the sample rack from being damaged by exposure to the atmosphere.

[0056] like Figure 7 and Figure 8 As shown, the sample fine-tuning system 200 is fed into the vacuum chamber 100 from the eleventh flange interface 11 at the top. Figure 9 As shown, the sample fine-tuning system 200 includes, arranged in order from bottom to top, a multi-sample holder 210, a horizontal motor 220, a vertical motor 230, and a rotary motor 240. In this embodiment, the horizontal motor 220 is mounted on the vacuum chamber 100, the vertical motor 230 is mounted on the movable platform of the horizontal motor 220, and the rotary motor 240 is mounted on the movable platform of the vertical motor 230.

[0057] The multi-sample holder 210 has numerous sample mounting slots 311, allowing for simultaneous mounting of multiple samples for batch experiments. A horizontal motor 220 provides two orthogonal dimensions of motion within the horizontal plane, allowing for movement of the multi-sample holder within the horizontal plane. A vertical motor 230 provides vertical movement of the multi-sample holder. A rotary motor 240 provides rotational control of the multi-sample holder 210 within the horizontal plane.

[0058] In addition, the sample fine-tuning system 200 also includes a bellows 250 that cooperates with the horizontal motor 220, the vertical motor 230 and the rotary motor 240 and is sealed with the vacuum experimental chamber 100. Thus, the motor is installed outside the vacuum, in the atmospheric environment, to drive the bellows to move horizontally, up and down, and rotate. The bellows 250 provides the dimension of motor movement and seals the vacuum at the same time. Thus, the vacuum is sealed and a large movement range is provided through the motor outside the vacuum to drive the movement of the equipment inside the vacuum.

[0059] The specific structure of the support platform 500 is as follows: Figure 1 and Figure 10 As shown. The entire vacuum test chamber 100, the vacuum control system 400 and the pump group matched with the vacuum control system 400 are fixed as shown. Figure 10 On the support platform 500 shown.

[0060] like Figure 1 and Figure 10 As shown, the support platform 500 includes an upper platform 501 and a lower platform 502. The upper platform 501 is an optical platform with M5 screw holes spaced 5 cm x 5 cm apart, used to secure the vacuum chamber 100 and its associated experimental equipment (including cameras, lighting, fluorescence detection system 300, etc.). The lower platform 502 is a metal partition used to place and secure related equipment and experimental instruments, such as the vacuum pump of the vacuum control system 400, as well as other subsequent test instruments.

[0061] The support platform 500 also includes an adapter plate 503, to which the vacuum chamber 100 is fixed via the support legs 14 on the columnar tube 12. The adapter plate 503 is fixed to the upper storage platform 501 via adapter plate fixing screws 504. The adapter plate 503 is provided with four ejector pins 505 and four pressure plates 506. The ejector pins 505 and pressure plates 506 are both fixed to the upper storage platform 501 and each is provided with a horizontally retractable screw. By rotating the screw, the end of the screw can be horizontally retracted relative to the ejector pins 505 and pressure plates 506, thereby pushing the vacuum chamber 100 horizontally. The ejector pins 505 and pressure plates 506 push the vacuum chamber 100 in two opposing directions, thereby limiting the horizontal position of the vacuum chamber 100. Therefore, after loosening the adapter plate fixing screws 504 and the four pressure plates 506, by adjusting the four ejector pins 505, the vacuum chamber 100 can be slightly translated along the adjustment direction of the ejector pins 505 and the pressure plates 506 and slightly adjusted in angle around the central axis of the adapter plate, ensuring that X-rays can pass through the light entrance of the vacuum chamber 100 to irradiate the sample at the center of the vacuum chamber 100, while the transmitted X-rays can enter the subsequent detection system through the light exit window of the vacuum chamber 100.

[0062] like Figure 11 As shown, the fluorescence detection system 300 includes a fluorescence detector 310, a motion motor 320 arranged below the fluorescence detector 310, a detection system bellows 330 connected between the fluorescence detector 310 and the vacuum experimental chamber 100, and a motor bracket 340 arranged between the motion motor 320 and the support platform 500.

[0063] Among them, the fluorescence detector 310 includes a fluorescence detector host 311 and a fluorescence detector probe 312. The fluorescence detector probe 312 is connected to the first flange interface 1 of the vacuum experimental chamber 100 via the detection system bellows 330. As a result, the fluorescence detector probe 312 is in a vacuum to eliminate air interference; the fluorescence detector host 311 is in the atmospheric environment outside the vacuum to facilitate heat dissipation. The motion motor 320 is used to provide one-dimensional movement to control the distance between the fluorescence detector probe 312 and the multi-sample holder 210 of the sample fine-tuning system 200 for quantitative experiments. The motor bracket 340 is used to assemble the motion motor 320 on the support platform 500 and provide a coarse adjustment function, which can roughly align the movement direction of the motion motor 320 with the multi-sample holder 210 of the sample fine-tuning system 200.

[0064] The vacuum control system 400 includes a vacuum pump 401 and multiple vacuum pipes 402 connected between the vacuum chamber 100 and the vacuum pump 401 to achieve vacuuming. The multiple vacuum pipes 402 are equipped with electric valves with different pumping speeds, and all the electric valves are connected to a switch controller, which ensures that the pumping speeds of the multiple vacuum pipes 402 are different. The switch controller is configured to open and close the different vacuum pipes 402 to achieve a slow pumping speed followed by a fast pumping speed during vacuuming, thus providing a window protection function. This effectively reduces the impact of the pressure difference generated during vacuuming / breaking of the vacuum chamber 100 on the thin Be window between the X-ray optical path and the vacuum chamber 100. Furthermore, the switch controller can be used to perform vacuuming / breaking operations with a single button, allowing the vacuum chamber 100 to quickly reach a testable state (within 5 minutes), reducing operational complexity and avoiding the serious consequences of misoperation.

[0065] like Figure 12 and Figure 13 As shown, the vacuum chamber 100 is further provided with a signal enhancement system 110, which includes a bias ring 111 fixed in the main body of the vacuum chamber 100, a first vacuum electrical feedthrough 112 electrically connected to the bias ring 111, and a positive voltage power supply (not shown) outside the chamber and connected to the first vacuum electrical feedthrough 112.

[0066] The first vacuum electrical feedthrough 112 is installed on the tenth flange interface 10 , and uses a SHV (high voltage coaxial feedthrough) connector to implement electrical feedthrough, and is electrically connected to the bias ring 111 via an anti-static wire 113 .

[0067] The bias ring 111 is in the shape of a circular ring and is made of pure copper, with an inner diameter of 50 mm, an outer diameter of 70 mm, and a thickness of 2 mm. The bias ring 111 is fixed to the inner wall surface of the vacuum test chamber 100 by three ceramic columns 114 to ensure that the bias ring 111 is insulated from the vacuum test chamber 100. The central axis of the bias ring 111 is collinear with the central axis of the vacuum test chamber 100 and is aligned with the multi-sample holder 210 of the sample fine-tuning system 200. The distance from the center of the bias ring 111 to the center of the sphere of the vacuum test chamber 100 is 100 mm. This size and distance design ensures that the outer side of the bias ring 111 will not block the X-rays, and the inner diameter of the bias ring 111 will not obstruct the line of sight of the camera. Among them, the bias ring 111 is arranged at a position close to the second flange interface 2. That is, the front face of the multi-sample holder 210 forms a 45° angle with the central axis of the third flange interface 3 (i.e., the incident flange), thereby receiving X-rays incident at a 45° angle, and the front face of the multi-sample holder 210 faces the bias ring 111, i.e., the front face of the multi-sample holder 210 is parallel to the surface of the bias ring 111.

[0068] In the signal enhancement system, an external positive voltage power supply is connected to the bias ring 111 through a first vacuum feedthrough 112 to form a high-voltage circuit. During use, a positive voltage of approximately 200V is applied to the bias ring, introducing an electric field between the bias ring and the sample. Secondary electrons generated by excitation on the sample surface are captured by the bias ring 111 under the action of this electric field. This reduces the number of effective low-energy Auger electrons on the sample surface that are unable to be promptly extracted and thus undergo coincidence or annihilation, effectively enhancing the signal-to-noise ratio of the TEY test.

[0069] The multi-sample holder 210 is a sample holder system, which includes a sample rod 311 fixed on the eleventh flange interface 11 on the top of the vacuum test chamber 100, an insulating block 312 installed on the sample rod 311, a metal sample rack 313 fixed by the insulating block 312, and a sample holder 314, which is used to install multiple samples.

[0070] In this embodiment, the insulating block 312 is made of ceramic, and the metal sample holder 313 is made of pure copper. The metal sample holder 313 is made of pure copper and has an inverted U-shape. It has a screw on the top that matches the insulating block 312 and three slots on the bottom for securing the sample holder. Thus, the sample is connected to the external test circuit via the metal sample holder 313 and the second vacuum feedthrough in the multi-sample holder 210, forming a TEY test loop. The output signal of the second vacuum feedthrough serves as the TEY test signal.

[0071] An antistatic wire is also provided between the metal sample holder 313 of the multi-sample rack 210 and the second vacuum feedthrough at the upper end of the sample rod 311. One end of the antistatic wire is fixed to the metal sample holder 313 via a terminal 315, and the other end is connected to the second vacuum feedthrough with a BNC interface at the upper end of the sample rod 311 in the vacuum test chamber 100. The exterior of the second vacuum feedthrough is connected to an external test circuit (not shown). The signal drawn from the sample by the second vacuum feedthrough serves as the TEY test signal. The middle portion of the second vacuum feedthrough and its mounting location are insulated, so it can be installed anywhere on the vacuum motor in the sample fine-tuning system 200 (for example, on the flange of the horizontal motor 220), be included with the vacuum motor, or be installed on other flange interfaces in the vacuum test chamber 100.

[0072] The vacuum chamber 100 is grounded, and the multi-sample holder 210 and the vacuum chamber 100 as well as the bias ring 111 and the vacuum chamber 100 are isolated by ceramic insulating blocks to prevent short circuits and form voltage conditions similar to those of Figure 14The high-voltage circuit is similar to that of the flat-plate ionization chamber shown in the figure. The voltage conditions are similar to those of the flat-plate ionization chamber, meaning that the vacuum chamber 100 corresponds to the outer shell of the flat-plate ionization chamber, the bias ring 111 corresponds to the high-voltage electrode of the flat-plate ionization chamber, and the metal sample holder 313 in the multi-sample holder 210 corresponds to the collector electrode of the flat-plate ionization chamber. Therefore, the bias ring 111 does not generate a test signal; it is used to capture electrons and maintain the electric field. After the sample loses electrons, it is connected to the outside world through a second vacuum feedthrough to generate a TEY test signal.

[0073] Sample holder 314 is made of pure aluminum or copper. Three protrusions on the top of sample holder 314 match the slots on the metal sample holder 313, securing the sample holder to the holder. This attachment method allows for one-handed operation. Sample holder 314 also has 2 x 10 8 mm x 12 mm through-holes for mounting samples and is X-ray transparent.

[0074] The above description is merely a preferred embodiment of the present invention and is not intended to limit the scope of the present invention. Various modifications are possible. Any simple, equivalent changes and modifications made in accordance with the claims and description of the present invention are within the scope of protection of the patent claims. Anything not fully described in this invention is conventional technology.

Claims

1. A vacuum spectroscopy test system, characterized in that: It includes a supporting platform, a vacuum experiment chamber and a fluorescence detection system adjacent to each other and all installed on the supporting platform, a vacuum control system, and a sample fine adjustment system installed above the vacuum experiment chamber; The sample fine-tuning system includes a multi-sample holder, a horizontal motor, a vertical motor, and a rotary motor arranged in sequence from bottom to top; an anti-static wire is provided between the metal sample holder of the multi-sample holder and the second vacuum feedthrough; the output signal of the second vacuum feedthrough is used as the TEY test signal; The vacuum test chamber is also provided with a signal enhancement system, which includes a bias ring fixed in the main body of the vacuum test chamber, a first vacuum electrical feedthrough electrically connected to the bias ring, and a positive pressure power supply outside the chamber connected to the first vacuum electrical feedthrough.

2. The vacuum spectroscopy testing system according to claim 1, characterized in that: The main body of the vacuum test chamber is spherical, with an outer diameter of 300 mm and a wall thickness of 3 mm, and a plurality of flange interfaces are symmetrically distributed on the main body.

3. The vacuum spectroscopy testing system according to claim 2, characterized in that: The vacuum test chamber satisfies at least one of the following: a1) One of the flange interfaces is connected to the upstream X-ray optical path using a Be window; a2) The outside of the vacuum test chamber is provided with an illumination lamp aligned with one of the flange interfaces and a camera aligned with one of the flange interfaces; a3) one of the flange interfaces is provided with a first vacuum electrical feedthrough and one of the flange interfaces is provided with a second vacuum electrical feedthrough; a4) A waste sample cleaning chamber is installed at the lower end of the vacuum test chamber. One end of the waste sample cleaning chamber is connected to a vacuum pump, and the other end is provided with a vacuum flange and a cleaning mask. A vacuum valve is installed between the vacuum test chamber and the waste sample cleaning chamber; a5) A cylindrical tube is provided at the bottom of the vacuum test chamber. The cylindrical tube is provided with two thirteenth flange interfaces for connecting to the exhaust control system and four supporting feet. The fixing feet are used to fix the vacuum test chamber to the supporting platform.

4. The vacuum spectroscopy testing system according to claim 1, characterized in that: The sample fine adjustment system further comprises a bellows which cooperates with the horizontal motor, the vertical motor and the rotary motor and is sealed with the vacuum experimental chamber.

5. The vacuum spectroscopy testing system according to claim 1, characterized in that: The support platform includes an upper storage platform and a lower storage platform. The upper storage platform is an optical platform with M5 screw holes with a spacing of 5cm×5cm, which is used to fix the vacuum experimental chamber. The lower storage platform is a metal partition for placing and fixing related equipment and experimental instruments.

6. The vacuum spectroscopy testing system according to claim 5, characterized in that: The support platform also includes an adapter plate, the vacuum test chamber is fixed on the adapter plate, and the adapter plate is fixed to the upper storage table by adapter plate fixing screws; four ejectors and four pressing plates are provided on the adapter plate, and the ejectors and pressing plates are both fixed on the upper storage table and are each provided with a horizontally retractable screw.

7. The vacuum spectroscopy testing system according to claim 1, characterized in that: The fluorescence detection system includes a fluorescence detector, a motion motor arranged below the fluorescence detector, a detection system bellows connected between the fluorescence detector and the vacuum experimental chamber, and a motor bracket arranged between the motion motor and the support platform.

8. The vacuum spectroscopy testing system according to claim 1, characterized in that: The vacuum control system includes a vacuum pump and multiple vacuum pipes connected between the vacuum experimental chamber and the vacuum pump; the multiple vacuum pipes are provided with electric valves with different pumping speeds, and all the electric valves are connected to a switch controller; the switch controller is configured to open and close different vacuum pipes to achieve slow pumping first and then fast pumping during pumping, thereby realizing the window protection function.

9. The vacuum spectroscopy testing system according to claim 1, characterized in that: The bias ring is in the shape of a circular ring and is made of pure copper with an inner diameter of 50 mm, an outer diameter of 70 mm, and a thickness of 2 mm. The bias ring is fixed to the inner wall of the vacuum test chamber by three ceramic columns. The central axis of the bias ring is collinear with the central axis of the vacuum test chamber and is aligned with the multi-sample holder of the sample fine-tuning system. The distance from the center of the bias ring to the center of the sphere of the vacuum test chamber is 100 mm.

10. The vacuum spectroscopy testing system according to claim 1, characterized in that: The multi-sample holder comprises a sample rod fixed on an eleventh flange interface on the top of the vacuum chamber, an insulating block mounted on the sample rod, a metal sample rack fixed by the insulating block, and a sample tray for mounting multiple samples.

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