A local high pressure air inlet device for a laval nozzle suitable for near normal pressure photoelectron spectrometer and application

Abstract

The present application relates to a kind of local high pressure intake device of Laval nozzle suitable for near normal pressure photoelectron spectroscopy and application.Laval nozzle intake device includes sequentially connected flowmeter intake pipeline, angle valve, four-way flange, pipe body and Laval nozzle along the direction of gas passing;Linear drive unit for adjusting the position of Laval nozzle in Z direction and XY displacement table for adjusting the position of Laval nozzle in XY plane are sequentially set on the pipe body, linear drive unit is connected with four-way flange by double flange, pipe body is connected with double flange, XY displacement table and linear drive unit are connected by collimator;Straight flange is provided on the side of XY displacement table away from collimator;It also includes diaphragm gauge, and diaphragm gauge is communicated with four-way flange.The design of the present application can make high-speed airflow hit on sample surface, so as to form local high pressure on surface, and the chemical state and electronic structure of sample surface in reaction atmosphere can be accurately characterized in situ.

Description

Technical Field

[0001] This invention relates to the field of in-situ spectroscopic characterization technology, and in particular to a Laval nozzle local high-pressure inlet device and its application suitable for near-normal pressure photoelectron spectroscopy. Background Technology

[0002] X-ray photoelectron spectroscopy (XPS) is one of the primary tools for studying the chemical composition of surfaces. The inherent surface sensitivity of this technique stems from the short mean free path of electrons within the material, typically only a few nanometers in size. Therefore, XPS is widely used to study the interactions between molecules and surfaces. It provides a wealth of information for the well-controlled and systematic study of single-crystal surfaces under ultra-high vacuum conditions. Traditionally, the application of XPS in more realistic systems, such as solid-liquid and solid-gas interfaces under high pressure, has been limited due to the strong inelastic scattering of photoemitted electrons. However, the most important heterogeneous catalytic reactions typically occur under high pressure and high temperature. Using differential pumping systems, electrostatic lenses, and capillary cones, pressure differences of several orders of magnitude can be achieved between the region surrounding the sample and the first differential pumping stage, enabling in-situ XPS characterization of catalytic reactions, i.e., near-atmospheric pressure photoelectron spectroscopy (AP-XPS). AP-XPS allows for real-time monitoring of dynamic changes in samples under controlled atmospheric conditions (such as high temperature and high pressure), particularly useful for studying catalytic reaction mechanisms, surface modification of thin film materials, and in-situ analysis of electrochemical processes. However, precise control of the reactant gas in a near-ambient pressure environment is a significant challenge during in-situ characterization. Importantly, in actual catalytic environments, the atmosphere over the catalyst surface is constantly flowing and at relatively high pressure. To closely mimic the actual catalytic environment, it is necessary to maintain atmospheric flow and maximize the pressure in the sample testing area. Controlling the gas flow rate and pressure in the reaction zone on the sample surface will greatly influence the in-situ characterization results.

[0003] Conventional gas inlet devices for near-atmospheric pressure photoelectron spectroscopy in existing technologies, such as Figure 1 As shown, in the in-situ characterization chamber 12 (which is a near-atmospheric pressure chamber), gas is delivered to the catalyst surface inside the chamber through a micro-leakage valve 11. Under certain pressure and catalyst temperature, the atoms on the catalyst surface interact with the gas molecules of the reactant gas, resulting in a chemical reaction that produces new substances and new catalyst surface structures. Under the action of X-rays, the core energy level electrons of the gaseous species on the material surface are excited; the kinetic energy of the excited electrons is obtained by an electron energy analyzer, thereby obtaining information on the chemical state and electronic structure of the material surface.

[0004] To control the atmospheric flow rate on the sample surface and increase the atmospheric pressure in the sample testing area, this invention designs a Laval nozzle high-pressure inlet device and integrates it into a near-atmospheric pressure photoelectron spectroscopy system. This enables in-situ dynamic characterization of the catalyst surface in an atmosphere. Summary of the Invention

[0005] In view of the shortcomings of the prior art described above, the purpose of this invention is to provide a Laval nozzle local high-pressure gas inlet device suitable for near-atmospheric pressure photoelectron spectroscopy. By adjusting the spatial position of the nozzle in the chamber through a collimator, a linear drive unit, and an XY displacement stage, the gas flow rate and pressure in the vicinity of the sample can be controlled. This design enables high-speed gas flow to hit the sample surface, thereby forming a local high pressure on the surface. It can accurately characterize the chemical state and electronic structure of the sample surface in the reaction atmosphere, thus solving the problems in the prior art.

[0006] To achieve the above and other related objectives, the present invention provides a local high-pressure gas inlet device for a Laval nozzle suitable for near-normal pressure photoelectron spectroscopy. The device includes a flow meter inlet pipe, an angle valve, a four-way flange, a pipe body, and a Laval nozzle connected sequentially along the gas flow direction. A linear drive unit for adjusting the position of the Laval nozzle in the Z direction and an XY displacement stage for adjusting the position of the Laval nozzle in the XY plane are sequentially mounted on the pipe body. The linear drive unit is connected to the four-way flange via a double-sided flange, and the pipe body is connected to the double-sided flange. The XY displacement stage and the linear drive unit are connected via a collimator. A straight-through flange is provided on the side of the XY displacement stage away from the collimator. The device also includes a diaphragm gauge, which communicates with the four-way flange.

[0007] In some embodiments of the present invention, the Laval nozzle includes a connected nozzle body and a nozzle outlet. The nozzle body is connected to the tube body. The inner diameter of the nozzle body gradually decreases from one end near the tube body to one end near the nozzle outlet, and the inner diameter of the nozzle outlet gradually increases from one end near the nozzle body to one end away from the nozzle body.

[0008] In some embodiments of the present invention, the nozzle body includes a proximal end and a distal end, the inner diameter of the proximal end of the body is smaller than the inner diameter of the tube body, the inner diameter of the proximal end of the body is larger than the inner diameter of the distal end of the body, the inner diameter of the distal end of the body is equal to the inner diameter of the proximal end of the outlet, and the inner diameter of the distal end of the outlet is larger than the inner diameter of the proximal end of the outlet.

[0009] In some embodiments of the present invention, the inner diameter of the tube is 5-7 mm.

[0010] In some embodiments of the present invention, the inner diameter of the proximal end of the body is 2 to 4 mm.

[0011] In some embodiments of the present invention, the inner diameters of the distal end of the body and the proximal end of the outlet are both 0.08 to 0.24 mm.

[0012] In some embodiments of the present invention, the inner diameter of the distal end of the outlet is 0.15 to 0.5 mm.

[0013] In some embodiments of the present invention, the angle α between the sidewall of the nozzle outlet and its axis is 5° to 15°.

[0014] In some embodiments of the present invention, the linear drive unit includes a bellows and a drive section for driving the bellows to extend and retract.

[0015] In some embodiments of the present invention, the stroke of the linear drive unit is 0 to 100 mm.

[0016] In some embodiments of the present invention, the Y-displacement stage includes a fixed stage and a movable stage that can move relative to the fixed stage, the movable stage being connected to the collimator, and the fixed stage being connected to the through flange.

[0017] In some embodiments of the present invention, the travel of the XY displacement stage in the X direction is ±7mm, and the travel of the XY displacement stage in the Y direction is ±7mm.

[0018] In some embodiments of the present invention, the collimator includes two flanges, one of which is connected to a linear drive unit and the other flange is connected to an XY displacement stage; a plurality of telescopic rods are provided between the two flanges.

[0019] In some embodiments of the present invention, the tilt angle of the collimator is adjusted to ±5°.

[0020] This invention also provides a method of using the Laval nozzle localized high-pressure inlet device for near-atmospheric pressure photoelectron spectroscopy as described above, the method of use comprising:

[0021] 1) Place at least part of the tube body and Laval nozzle in the in-situ characterization chamber of the Laval nozzle inlet device. Gas enters the in-situ characterization chamber through the flow meter inlet pipe and the angle valve inlet four-way flange, and then enters the in-situ characterization chamber through the tube body and Laval nozzle in sequence.

[0022] 2) The position in the XY plane is adjusted by the XY displacement stage, the position in the Z direction is adjusted by the linear drive unit, and the angle is adjusted by the collimator, thereby accurately controlling the position of the Laval nozzle near the sample.

[0023] The present invention also provides an in-situ photoelectron spectroscopy characterization device, including a Laval nozzle local high-pressure inlet device as described above for near-ambient pressure photoelectron spectroscopy, and an in-situ characterization experimental chamber, wherein a sample is placed in the in-situ characterization experimental chamber, and the Laval nozzle inlet device is inserted through the side wall of the in-situ characterization experimental chamber and the Laval nozzle is close to the sample.

[0024] This invention provides a Laval nozzle inlet device and an in-situ photoelectron spectroscopy characterization device suitable for in-situ spectroscopic characterization, which have the following advantages:

[0025] (1) The Laval nozzle used in this invention can increase the high-speed flow rate of gas (e.g., 200 m / s) and directly hit the test area of ​​the sample in the chamber used for in-situ characterization experiment.

[0026] (2) The XY displacement stage, collimator and linear drive unit used in this invention can accurately adjust the angle and spatial position of the Laval nozzle in the chamber.

[0027] (3) In this invention, the gas flows towards the sample surface, forming a local high-pressure zone. To reduce gas phase scattering, the nozzle tip points directly at the sample while maintaining a relatively low chamber pressure. The nozzle employs a Laval nozzle structure, enabling the ejection of gas at higher velocities. This increases the local gas concentration and velocity near the sample, thereby achieving accurate in-situ characterization. Attached Figure Description

[0028] Figure 1 It is the ventilation method for near-normal pressure photoelectron spectroscopy in existing technology.

[0029] Figure 2 This is a three-dimensional structural schematic diagram of the Laval nozzle local high-pressure air intake device applicable to near-normal pressure photoelectron spectroscopy according to the present invention.

[0030] Figure 3 This is a schematic diagram of the structure of the in-situ photoelectron spectroscopy characterization device of the present invention.

[0031] Figure 4 This is a schematic diagram of the structure of the Laval nozzle of the present invention.

[0032] Figure 5 This is a schematic cross-sectional view of the Laval nozzle of the present invention.

[0033] Component reference numerals in the figures of this invention:

[0034] 1. Flow meter inlet pipe

[0035] 2 Angle valve

[0036] 3 Four-way flange

[0037] 4. Thin Film Specifications

[0038] 5 Double-sided flange

[0039] 6 Linear Drive Units

[0040] 61 Corrugated Pipe

[0041] 62 Drive Unit

[0042] 7. Collimator

[0043] 71 Flange

[0044] 72 Telescopic pole

[0045] 8 XY displacement stage

[0046] 81 Fixed platform

[0047] 82 mobile stations

[0048] 9 Straight-through flange

[0049] 10 Laval nozzles

[0050] 101 Nozzle Body

[0051] 1011 Proximal end of the body

[0052] 1012 Remote end of the main body

[0053] 102 Nozzle outlet

[0054] 1021 Near-end of exports

[0055] 1022 Export Remote

[0056] 11. Micro-leakage valve

[0057] 12. Chambers for in-situ characterization experiments

[0058] 13 tube body Detailed Implementation

[0059] In the description of this invention, it should be noted that the structures, proportions, sizes, etc., illustrated in the accompanying drawings are merely for illustrative purposes to aid those skilled in the art and to facilitate understanding and reading. They are not intended to limit the implementation conditions of this invention and therefore have no substantial technical significance. Any modifications to the structure, changes in proportions, or adjustments to size, without affecting the effects and objectives achieved by this invention, should still fall within the scope of the technical content disclosed in this invention. Furthermore, the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings. They are merely for the convenience of describing this invention 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. Therefore, they should not be construed as limitations on this invention. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0060] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" 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 invention according to the specific circumstances.

[0061] Furthermore, in the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0062] Example 1

[0063] like Figures 2-4As shown, this invention provides a Laval nozzle localized high-pressure gas inlet device suitable for near-ambient pressure photoelectron spectroscopy. Localized high pressure refers to the formation of a high-pressure region on the sample surface directly opposite the high-speed gas flow when gas exits the Laval nozzle at a relatively high rate. The device includes a flowmeter inlet pipe 1, an angle valve 2, a four-way flange 3, a pipe body 13, and a Laval nozzle 10 connected sequentially along the gas flow direction. The gas flow direction refers to the direction in which gas generated by an external gas generator passes through the flowmeter inlet pipe 1, angle valve 2, four-way flange 3, pipe body 13, and Laval nozzle 10 before finally entering the in-situ characterization experimental chamber. Specifically, gas enters the four-way flange 3 through the flowmeter inlet pipe 1 and angle valve 2. The inlet flow rate is controlled by adjusting the opening size of angle valve 2, thereby controlling the pressure within the four-way flange 3. The gas then passes through angle valve 2, sequentially entering the pipe body 13 and Laval nozzle 10 before entering a designated location within the in-situ characterization experimental chamber.

[0064] In the Laval nozzle air intake device provided in this embodiment of the invention, the angle valve 2 can be, for example, a metal angle valve 2, used to regulate the amount of gas entering the four-way flange 3, the pipe body 13 and the Laval nozzle 10 and finally entering the in-situ characterization experimental chamber 12.

[0065] In the Laval nozzle air intake device provided in the embodiments of the present invention, such as Figure 2 The four-way flange 3, in addition to being connected to the angle valve 2 and the pipe body 13 respectively, is also connected to the diaphragm gauge 4 for measuring the gas pressure inside the pipe body 13. In one specific embodiment, the diaphragm gauge 4 may be, for example, a Pfeffier CMR361 model.

[0066] In the Laval nozzle air inlet device provided in this embodiment of the invention, the pipe body 13 can be, for example, a stainless steel pipe. The pipe body 13 is connected to the four-way flange 3. Figure 2 A double-sided flange 5 is provided between the pipe body 13 and the four-way flange 3, and the four-way flange 3 and the double-sided flange 5 are threaded together. The pipe body 13 and the double-sided flange 5 are fixedly connected, for example, by welding.

[0067] In the Laval nozzle air inlet device provided in this embodiment of the invention, the Laval nozzle 10 is used to increase the speed of the introduced gas and to hit the sample surface with as much gas as possible.

[0068] Furthermore, such as Figure 4 The Laval nozzle 10 includes a connected nozzle body 101 and a nozzle outlet 102. The nozzle body 101 is connected to the tube 13. The inner diameter of the nozzle body 101 gradually decreases from one end near the tube 13 to one end near the nozzle outlet 102, and the inner diameter of the nozzle outlet 102 gradually increases from one end near the nozzle body 101 to one end away from the nozzle body 101.

[0069] like Figure 4 The Laval nozzle 10 includes a nozzle body 101 and a nozzle outlet 102. The nozzle body 101 is conical and includes a proximal end 1011 and a distal end 1012. The inner diameter of the proximal end 1011 is smaller than the inner diameter of the tube body 13, and the inner diameter of the proximal end 1011 is larger than the inner diameter of the distal end 1012. The inner diameter of the distal end 1012 is equal to the inner diameter of the proximal end 1021 of the outlet, and the inner diameter of the distal end 1022 of the outlet is larger than the inner diameter of the proximal end 1021 of the outlet.

[0070] Further optionally, the inner diameter of the tube body 13 is 5-7 mm. It can be 5-6 mm or 6-7 mm. The inner diameter of the proximal end 1011 of the body is 2-4 mm, and can be 2-3 mm or 3-4 mm. The inner diameters of the distal end 1012 of the body and the proximal end 1021 of the outlet are both 0.08-0.24 mm, and can be 0.08-0.2 mm or 0.2-0.24 mm. The inner diameter of the distal end 1022 of the outlet is 0.15-0.5 mm, and can be 0.15-0.4 mm or 0.4-0.5 mm.

[0071] Further optional, such as Figure 4 The included angle α between the sidewall of the nozzle outlet 102 and its axis is 5° to 15°. It can be selected as 5° to 8° or 8° to 15°.

[0072] The advantage of being within the aforementioned inner diameter and included angle range is that it ensures that the airflow at the outlet is high-speed and collimated to hit the sample testing area, thereby achieving local high pressure, such as 5-100 mbar. The disadvantage of being outside this range is that it cannot guarantee that the local pressure of the sample testing section will reach the optimal level.

[0073] In the Laval nozzle air intake device provided in the embodiments of the present invention, such as Figure 2 and 3A linear drive unit 6 for adjusting the position of the Laval nozzle 10 in the Z direction is fitted onto the tube body 13. The linear drive unit 6 is connected to the four-way flange 3 via a double-sided flange 5. The linear drive unit 6 can adjust the stroke of the Laval nozzle 10 in the Z direction into the in-situ characterization chamber. The stroke of the linear drive unit 6 is typically 0–100 mm, preferably 100 mm. The fully compressed state is 0 mm. In one embodiment, the linear drive unit 6 includes a bellows 61 and a drive part 62 for driving the bellows 61 to extend and retract. The drive part 62 includes a support rod and a drive rod that can slide relative to the support rod. The drive rod is connected to the bellows 61, and the double-sided flange 5 is then fixed to the entire linear drive unit 6 by screws. The drive rod drives the bellows to reciprocate and extend. In a specific embodiment, the linear drive unit 6 may be, for example, model LSM38-100-H (UHVDesign Ltd.), and a scale is provided on the linear drive unit 6 for measuring the stroke.

[0074] In the Laval nozzle air intake device provided in the embodiments of the present invention, such as Figure 2 and 3 The tube body 13 is also fitted with an XY displacement stage 8 for adjusting the position of the Laval nozzle 10 in the XY plane. The XY displacement stage 8 allows adjustment of the stroke of the Laval nozzle 10 into the in-situ characterization chamber 12 in both the X and Y directions. The stroke of the XY displacement stage 8 in the X direction is ±7mm, and the stroke in the Y direction is ±7mm. Taking a stroke of ±7mm in the X direction as an example, the center of the XY displacement stage 8 is 0. Moving 7mm to the right along the X direction from the center results in +7mm, and moving 7mm to the left along the X direction from the center results in -7mm. The stroke in the Y direction is explained similarly. In one specific embodiment, the XY displacement stage 8 can be, for example, a Fermi XY35. A straight flange 9 is provided on the side of the XY displacement stage 8 away from the collimator 7, connecting the Laval nozzle air inlet device to the in-situ characterization chamber 12. The linear drive unit 6 and the XY displacement stage 8 are connected via the collimator 7. The XY displacement stage 8 includes a fixed stage 81 and a movable stage 82 that can move relative to the fixed stage 81. The fixed stage 81 is connected to the through flange 9, and the movable stage 82 is connected to the collimator 7. When the XY displacement stage 8 of the above model moves relative to the fixed stage 81 via the movable stage 82, the movable stage 82 drives the collimator 7, the linear drive unit 6, the tube body 13, and the Laval nozzle 10 to move as a whole in the XY plane.

[0075] In the Laval nozzle air intake device provided in the embodiments of the present invention, such as Figure 2The collimator 7 is used to adjust the angle of the Laval nozzle 10. The collimator 7 includes two flanges 71, with a telescopic tube (e.g., a bellows) between them. One flange 71 is connected to the linear drive unit 6, and the other flange 71 is connected to the XY displacement stage 8 (further connected to the moving stage 82 of the XY displacement stage 8). Multiple telescopic rods 72 are provided between the two flanges 71. By adjusting the distance and angle between the flanges 71 at both ends, for example, by simultaneously adjusting the axial distance of several telescopic rods 72, the axial distance of the Laval nozzle 10 intake device can be adjusted. Alternatively, adjusting the axial distance of one or two telescopic rods 72, with different adjustments, creates a tilt angle, thus adjusting the tilt angle. In one embodiment, by adjusting the distance and angle between the flanges 71 at both ends, the Laval nozzle intake device of the present invention can achieve a tilt angle adjustment of ±5°. The initial angle is 0° in its natural state, and the tilt angle is the angle of left-hand or right-hand rotation relative to the initial state after adjustment. In one specific embodiment, the collimator 7 may be, for example, a PA35-T (UHV Design Ltd.).

[0076] This invention also provides a method for using a Laval nozzle local high-pressure inlet device suitable for near-normal pressure photoelectron spectroscopy, comprising at least the following steps:

[0077] 1) Place at least part of the tube body 13 and Laval nozzle 10 in the in-situ characterization experimental chamber 12. Gas enters the four-way flange 3 through the flow meter inlet pipe 1 and the angle valve 2, and then enters the interior of the in-situ characterization experimental chamber 12 through the tube body 13 and Laval nozzle 10 in sequence.

[0078] 2) The position in the XY plane is adjusted by the XY displacement stage 8, the position in the Z direction is adjusted by the linear drive unit 6, and the angle is adjusted by the collimator 7, so as to accurately control the position of the Laval nozzle 10 near the sample.

[0079] Specifically: such as Figure 3As shown, the Laval nozzle inlet device is fixed to the in-situ characterization chamber 12 via a straight flange 9. Gas enters through a flow meter inlet pipe 1 and a metal angle valve 2 into a four-way flange 3. The four-way flange 3 is connected to a diaphragm gauge 4 and a double-sided flange 5. The metal angle valve 2 controls the gas flow rate. The gas entering the four-way flange 3 can further connect to the pipe body 13, and then to the Laval nozzle 10, entering the interior of the in-situ characterization chamber 12. The position of the Laval nozzle 10 inside the in-situ characterization chamber 12 can be adjusted by using an XY displacement stage 8 to adjust its in-plane position, by using a linear drive to adjust its Z-direction position, and by using a collimator 7 to adjust its angle. In this way, the position of the Laval nozzle 10 near the sample can be accurately controlled, thereby controlling the distribution of gas concentration and pressure near the sample. The shape of the Laval nozzle 10 used in this invention is specifically as shown below. Figure 4 As shown, the Laval nozzle 10 is connected to the tube body 13 and extends to the vicinity of the sample surface. This allows the gas exiting the Laval nozzle 10 to contact the sample surface as much as possible and maintain a certain flow rate, thereby increasing the local pressure. To control the pressure stability of the in-situ characterization chamber 12d, a mechanical pump (exhaust pump) is installed at the outlet of the in-situ characterization chamber 12. This allows for increased pumping speed at higher gas flow rates, thereby controlling the pressure stability inside the in-situ characterization chamber 12.

[0080] Example 2

[0081] like Figure 3 The present invention also provides an in-situ photoelectron spectroscopy characterization device, including the Laval nozzle local high-pressure inlet device suitable for near-normal pressure photoelectron spectroscopy as described in Embodiment 1, and an in-situ characterization experimental chamber 12, in which a sample is placed. The Laval nozzle inlet device is inserted into the side wall of the in-situ characterization experimental chamber 12 and the Laval nozzle 10 is close to the sample.

[0082] In one specific embodiment, the XY displacement stage 8 is mounted on the side wall of the in-situ characterization experimental chamber 12 via a through flange 9, and the side wall is provided with corresponding openings so that part of the tube body 13 and the Laval nozzle 10 can be located in the in-situ characterization experimental chamber 12. For the specific principle of the in-situ characterization experimental device, please refer to the patent , application number: 2024221786117.

[0083] When in use, the linear drive unit 6 can shorten or lengthen. Taking its gradual lengthening as an example: as the linear drive unit 6 gradually lengthens, it gradually pushes the four-way flange 3 and the flow meter inlet pipe 1, which are connected to it in sequence, away from the in-situ characterization chamber 12. When the flow meter inlet pipe 1 is pushed away from the in-situ characterization chamber 12, the pipe body 13 and the Laval nozzle 10, which are connected to the four-way flange 3 in sequence, will gradually move outward from the in-situ characterization chamber 12, and the Laval nozzle 10 will gradually move away from the sample. Similarly, when the linear drive unit 6 gradually shortens, the Laval nozzle 10 will gradually move closer to the sample. Therefore, the distance of the sample injection in the Z direction can be controlled by the linear drive unit 6.

[0084] In use, the XY displacement stage 8 includes a fixed stage 81 and a movable stage 82. The fixed stage 81 is connected to a straight flange 9, which is fixed to the side wall of the in-situ characterization chamber 12. The movable stage 82 is connected to the collimator 7. By moving the movable stage 82 relative to the fixed stage 81, the movable stage 82 drives the collimator 7, the linear drive unit 6, the tube body 13, and the Laval nozzle 10 to move as a whole in the XY plane. The XY displacement stage 8 allows for adjustment of the stroke of the Laval nozzle 10 extending into the in-situ characterization chamber 12 in the X and Y directions.

[0085] When in use, the collimator 7 adjusts the distance and angle between the flanges 71 at both ends. For example, when there are three telescopic rods, the axial distance of one or two telescopic rods 72 can be adjusted, and the adjusted distances can be different, while the third telescopic rod remains stationary, thereby creating a tilt angle and achieving the adjustment of the tilt angle.

[0086] In summary, the present invention provides a Laval nozzle inlet device and an in-situ photoelectron spectroscopy characterization device suitable for in-situ spectroscopic characterization, which have the following advantages:

[0087] (1) The Laval nozzle 10 used in this invention can provide high-speed airflow, which directly hits the test area of ​​the chamber sample for in-situ characterization experiment.

[0088] (2) The XY displacement stage 8, collimator 7 and linear drive unit 6 used in this invention can accurately adjust the angle and spatial position of the Laval nozzle 10 in the chamber.

[0089] (3) In this invention, the gas flows towards the sample surface, forming a local high-pressure zone. To reduce gas phase scattering, the nozzle tip points directly at the sample while maintaining the chamber pressure at a relatively low level. The nozzle adopts the structure of a Laval nozzle 10, which can eject gas at a higher flow rate. This can increase the local gas concentration and velocity near the sample, thereby achieving accurate in-situ characterization.

[0090] In summary, this invention effectively overcomes the various shortcomings of the prior art and has high industrial application value.

[0091] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

Claims

1. A Laval nozzle localized high-pressure inlet device suitable for near-atmospheric pressure photoelectron spectroscopy, characterized in that, The device includes a flow meter inlet pipe (1), an angle valve (2), a four-way flange (3), a pipe body (13), and a Laval nozzle (10) connected sequentially along the gas flow direction; the pipe body (13) is fitted with a linear drive unit (6) for adjusting the position of the Laval nozzle (10) in the Z direction and an XY displacement stage (8) for adjusting the position of the Laval nozzle (10) in the XY plane; the linear drive unit (6) is connected to the four-way flange (3) through a double-sided flange (5); the pipe body (13) is connected to the double-sided flange (5); the XY displacement stage (8) and the linear drive unit (6) are connected through a collimator (7); a straight flange (9) is provided on the side of the XY displacement stage (8) away from the collimator (7); it also includes a diaphragm gauge (4), which is connected to the four-way flange (3).

2. The Laval nozzle local high-pressure inlet device suitable for near-atmospheric pressure photoelectron spectroscopy as described in claim 1, characterized in that, The Laval nozzle (10) includes a connected nozzle body (101) and a nozzle outlet (102). The nozzle body (101) is connected to the tube (13). The inner diameter of the nozzle body (101) gradually decreases from one end near the tube (13) to one end near the nozzle outlet (102), and the inner diameter of the nozzle outlet (102) gradually increases from one end near the nozzle body (101) to one end away from the nozzle body (101).

3. The Laval nozzle local high-pressure inlet device suitable for near-normal pressure photoelectron spectroscopy as described in claim 2, characterized in that, The nozzle body (101) includes a proximal end (1011) and a distal end (1012). The inner diameter of the proximal end (1011) is smaller than the inner diameter of the tube body (13). The inner diameter of the proximal end (1011) is larger than the inner diameter of the distal end (1012). The inner diameter of the distal end (1012) is equal to the inner diameter of the outlet proximal end (1021). The inner diameter of the distal end (1022) is larger than the inner diameter of the outlet proximal end (1021).

4. The Laval nozzle local high-pressure inlet device suitable for near-normal pressure photoelectron spectroscopy as described in claim 2, characterized in that, The inner diameter of the tube (13) is 5-7 mm; And / or, the inner diameter of the proximal end (1011) of the body is 2 to 4 mm; And / or, the inner diameter of the distal end (1012) of the body and the proximal end (1021) of the outlet are both 0.08 to 0.24 mm; And / or, the inner diameter of the distal end of the outlet (1022) is 0.15 to 0.5 mm.

5. The Laval nozzle local high-pressure inlet device suitable for near-normal pressure photoelectron spectroscopy as described in claim 2, characterized in that, The angle α between the sidewall of the nozzle outlet (102) and its axis is 5° to 15°.

6. The Laval nozzle local high-pressure inlet device suitable for near-atmospheric pressure photoelectron spectroscopy as described in claim 1, characterized in that, The linear drive unit (6) includes a bellows (61) and a drive unit (62) for driving the bellows (61) to extend and retract. And / or, the stroke of the linear drive unit (6) is 0 to 100 mm.

7. The Laval nozzle local high-pressure inlet device suitable for near-atmospheric pressure photoelectron spectroscopy as described in claim 1, characterized in that, The Y-displacement stage includes a fixed stage (81) and a movable stage (82) that can move relative to the fixed stage (81). The movable stage (82) is connected to the collimator (7), and the fixed stage (81) is connected to the through flange (9). And / or, the XY displacement stage (8) has a travel of ±7mm in the X direction and a travel of ±7mm in the Y direction.

8. The Laval nozzle local high-pressure inlet device for near-atmospheric pressure photoelectron spectroscopy as described in claim 1, characterized in that, The collimator (7) includes two flanges (71), one of which is connected to the linear drive unit (6) and the other flange (71) is connected to the XY displacement stage (8); a plurality of telescopic rods (72) are provided between the two flanges (71); And / or, the tilt angle of the collimator (7) is adjusted to ±5°.

9. The method of using the Laval nozzle local high-pressure inlet device for near-atmospheric pressure photoelectron spectroscopy as described in any one of claims 1 to 8, characterized in that, The method of use includes: 1) Place at least part of the pipe body (13) and Laval nozzle (10) of the Laval nozzle air inlet device in the in-situ characterization experimental chamber (12). The gas enters the four-way flange (3) through the flow meter air inlet pipe (1) and the angle valve (2), and then enters the interior of the in-situ characterization experimental chamber (12) through the pipe body (13) and the Laval nozzle (10) in sequence. 2) The position in the XY plane is adjusted by the XY displacement stage (8), the position in the Z direction is adjusted by the linear drive unit (6), and the angle is adjusted by the collimator (7), so as to accurately control the position of the Laval nozzle (10) near the sample.

10. An in-situ photoelectron spectroscopy characterization device, characterized in that, The device includes a Laval nozzle local high-pressure inlet device for near-normal pressure photoelectron spectroscopy as described in any one of claims 1 to 8, and further includes an in-situ characterization experimental chamber (12) in which a sample is placed, wherein the Laval nozzle inlet device is inserted through the side wall of the in-situ characterization experimental chamber (12) and the Laval nozzle (10) is close to the sample.

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