A plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy

Abstract

The application provides a plasma spray gun device compatible with near-normal-pressure photoelectron spectroscopy, and relates to the field of in-situ spectroscopy characterization.The first aspect of the application provides a plasma spray gun device compatible with near-normal-pressure photoelectron spectroscopy, which can realize the synchronization of gas delivery and plasma generation at the same position, guarantee the uniformity of the plasma entering the chamber for in-situ characterization experiments, and can concentrate the plasma in the test area, so that the plasma concentration on the surface of the sample is increased, and the surface reaction of the sample is improved.The second aspect of the application provides an in-situ photoelectron spectroscopy characterization device.

Description

Technical Field

[0001] The present invention relates to the field of in-situ spectroscopy characterization, in particular to a plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy. Background Art

[0002] Plasma is the fourth state of matter, in addition to solid, liquid, and gas. The large number of ions, high-energy electrons, and excited atoms and molecules within it provide reactive groups that are prone to chemical reactions, allowing plasma-enhanced chemical transformation processes to exhibit unconventional behavior under specific external fields. Plasma is a cutting-edge development area of ​​global concern, with widespread applications in energy, environment, materials, chemical engineering, and other fields. Near-ambient-pressure photoelectron spectroscopy is crucial in scientific research, as it can observe and record reactions and material changes under realistic conditions. Its elemental and chemical specificity, high surface sensitivity, and ease of use facilitate in-depth study of the electronic geometry of materials, the atomic structure of the coordination environment, and morphological changes, allowing for the exploration of dynamic changes on the sample surface during reactions. This has greatly promoted the development of new materials, catalysts, and drugs, and is widely used in fields such as chemistry, materials science, and biology.

[0003] Plasma is a typical multidisciplinary field, and research is still relatively scarce. Near-normal pressure photoelectron spectroscopy technology can perform in-situ characterization of the chemical state and electronic structure of the material surface. It is widely used in catalytic reactions and semiconductor technology research. In semiconductor technology, most plasma processing processes have a pressure of 10 -1 ~10 3 The range of pa, which overlaps with the working pressure range of near-atmospheric pressure photoelectron spectroscopy, is beneficial to the study of the interaction between plasma and solid or liquid and the real-time monitoring of plasma process.

[0004] Traditional studies use non-in situ or quasi-in situ methods (for example, by treating the sample in a plasma environment and then vacuum transferring it to a test chamber for vacuum characterization), which cannot change the high vacuum environment during the characterization process. Although this helps to understand plasma-induced surface phenomena, it does not have the ability to perform in situ characterization of the surface chemical state and electronic structure changes of the sample in the plasma environment. This information is key to revealing the interaction mechanism between plasma and materials.

[0005] like Figure 1 As shown, in the in-situ characterization test chamber 10 (the chamber is a near-normal pressure chamber), gas is transported into the chamber through a micro-leak valve 1, and voltage is applied to the electrodes in the chamber by a high-voltage power supply to generate plasma and interact with the sample. Under the action of X-rays, atoms on the surface of the material, electrons of the reaction gas and plasma are excited; the kinetic energy of the excited electrons is obtained by the electron energy analyzer, and then information on the chemical state and electronic structure of the material surface is obtained.

[0006] However, the region where the plasma is generated is far away from the sample surface test region, the plasma concentration in the test region is low, the sample surface reaction is not obvious, and the plasma will react with the adsorbate on the chamber wall to produce many by-products, changing the sample surface results and affecting the research results. Therefore, designing a new type of plasma generation device suitable for in-situ photoelectron spectroscopy characterization is of great significance to the entire plasma in-situ characterization technology.

[0007] In view of the importance of plasma in-situ characterization technology to the development of material science and the importance of how to generate plasma to the plasma in-situ characterization technology, how to effectively generate plasma on the sample surface region and carry out in-situ characterization is a key technical problem that needs to be solved, which has a great influence on further promoting the development of material science. SUMMARY

[0008] To solve the above problems, the first aspect of the present application provides a plasma spray gun device compatible with near-normal pressure photoelectron spectroscopy, which can realize the synchronization of gas delivery and plasma generation at the same position, ensure the uniformity of the plasma entering the chamber for in-situ characterization experiment, and concentrate the plasma in the test region, so as to increase the plasma concentration on the sample surface and improve the surface reaction of the sample.

[0009] The first aspect of the present application provides a plasma spray gun device compatible with near-normal pressure photoelectron spectroscopy, which comprises a micro-leak valve connected with a gas generation device and a rear-end pipe, a middle-end pipe and a front-end pipe connected and communicated in sequence along the gas emission direction, the micro-leak valve is connected with and communicated with the rear-end pipe; further comprising a positive electrode lead-out pipe transversely arranged in the front-end pipe and the middle-end pipe, the head end and part of the positive electrode lead-out pipe are located in the front-end pipe, the tail end of the positive electrode lead-out pipe penetrates through the side wall of the middle-end pipe; the positive electrode lead-out pipe is provided with a positive electrode extension line; further comprising a positive electrode, a positive electrode lead-out positive electrode lead, a negative electrode and a negative electrode lead-out negative electrode lead; the positive electrode lead is connected with the positive electrode extension line and makes it conductive, and the negative electrode lead is connected with the front-end pipe and makes it conductive.

[0010] In some feasible embodiments, the length of the positive electrode lead-out pipe is 110-130 mm, the inner diameter is 1-2 mm, and the outer diameter is 2-3 mm; and / or, the length of the positive electrode extension line is 115-135 mm, and the diameter is 1-2 mm; and / or, the length of the front-end pipe is 90-110 mm, the inner diameter is 5-7 mm, and the outer diameter is 7-9 mm; and / or, the length of the middle-end pipe is 10-30 mm, the inner diameter is 2-4 mm, and the outer diameter is 3-5 mm; and / or, the length of the rear-end pipe is 550-570 mm, the inner diameter is 3-5 mm, and the outer diameter is 5.35-7.35 mm.

[0011] In an embodiment, the front-end tube is provided with a conductive tube and an insulating tube from outside to inside, and the insulating tube is nested on the outside of the middle-end tube; the conductive tube is provided with a negative electrode column, and the negative electrode lead is connected with the negative electrode column and makes it conductive; the positive electrode lead-out tube is also provided with a positive electrode column connected with the positive electrode extension line, and the positive electrode lead is connected with the positive electrode column and makes it conductive.

[0012] In some embodiments, the length of the conductive tube is 90-110 mm, the inner diameter is 4-6 mm, and the outer diameter is 5-7 mm; and / or, the length of the insulating tube is 86-106 mm, the inner diameter is 3-5 mm, and the outer diameter is 4-6 mm; and / or, the length of the negative electrode column is 2-4 mm, and the diameter is 1-2 mm; and / or, the length of the positive electrode column is 2-4 mm, and the diameter is 1-2 mm.

[0013] In some embodiments, one or more of the following technical features is included: 1) the head of the positive electrode extension line extends to the outside of the head end of the positive electrode lead-out tube; 2) the head end of the front-end tube extends to the outside of the head end of the conductive tube; 3) the head end of the conductive tube extends to the outside of the head end of the insulating tube.

[0014] In some embodiments, one or more of the following technical features is included: if the technical feature 1) in the above embodiment is included, the length of the head of the positive electrode extension line extending outward is 4-6 mm; if the technical feature 2) in the above embodiment is included, the length of the head end of the front-end tube extending outward is 4-6 mm; if the technical feature 3) in the above embodiment is included, the length of the head end of the conductive tube extending outward is 3-5 mm.

[0015] In an embodiment, it further includes a three-way valve, a collimator and a linear drive mechanism connected in sequence along the gas emission direction and all located outside the rear-end tube; the opposite ends of the three-way valve are connected with the collimator and the micro-leak valve respectively, and the positive electrode lead and the negative electrode pass through the three-way valve, the collimator and the linear drive mechanism in sequence; the linear drive mechanism is adapted to be connected with the side wall of the chamber for in-situ characterization experiments.

[0016] In some embodiments, the three-way valve is provided with an electrode flange on an independent end, and the positive electrode and the negative electrode are both arranged in the electrode flange; and / or, the axial angle adjustment of the collimator is ±5 mm, and the inclination angle adjustment is ±3°; and / or, the stroke of the linear drive mechanism is 90-110 mm.

[0017] The application also provides a use method of the plasma jet device compatible with the near-normal-pressure photoelectron spectrometer, which at least includes the following steps:

[0018] 1) gas passes through the micro leakage valve, in turn into the rear end tube, the middle end tube and the front end tube;

[0019] 2) the positive electrode and the negative electrode are energized, so that the positive electrode extension line connected with the positive electrode lead and the front end tube connected with the negative electrode lead are in a conductive state;

[0020] 3) the gas is ionized into plasma by the positive electrode extension line and the front end tube when passing through the front end tube.

[0021] The second aspect of the present application provides an in-situ photoelectron spectroscopy characterization device, comprising the plasma jet device compatible with near normal pressure photoelectron spectroscopy provided by the first aspect of the present application, characterized in that: further comprising an in-situ characterization experiment chamber, the in-situ characterization experiment chamber is suitable for placing a sample, and the plasma jet device is arranged in the side wall of the in-situ characterization experiment chamber and the head end of the front end tube is close to the sample.

[0022] The plasma jet device compatible with near normal pressure photoelectron spectroscopy and the in-situ photoelectron spectroscopy characterization device provided by the present application have the following beneficial effects:

[0023] 1) The plasma jet device compatible with near normal pressure photoelectron spectroscopy provided by the present application can realize the synchronization of gas delivery and plasma generation at the same position, ensure the uniformity of the plasma entering the in-situ characterization experiment chamber, and concentrate the plasma in the test area, so as to increase the plasma concentration on the surface of the sample and improve the surface reaction of the sample.

[0024] 2) The collimator and the linear drive mechanism in the plasma jet device compatible with near normal pressure photoelectron spectroscopy provided by the present application can rotate or stretch the plasma jet part in the characterization experiment chamber, so as to realize the regulation of the distance and angle between the plasma and the sample. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 It is a sample inlet device in the prior art.

[0026] Figure 2 It is a schematic diagram of the overall structure of the plasma jet device compatible with near normal pressure photoelectron spectroscopy of the present application.

[0027] Figure 3 It is a cross-sectional view of the front end tube, the middle end tube and the rear end tube of the present application.

[0028] Figure 4 It is a cross-sectional view of the front end tube, the conductive tube, the insulating tube, the positive electrode lead-out tube and the ionization region of the present application.

[0029] Figure 5 It is a cross-sectional view of the three-way valve, the collimator and the linear drive mechanism of the present application.

[0030] Figure 6 The figure is a schematic diagram of the overall structure of an in-situ photoelectron spectroscopy characterization device of the present invention.

[0031] Reference numerals

[0032] Micro-leakage valve 1

[0033] Rear end pipe 2

[0034] Middle end tube 3

[0035] Front end tube 4

[0036] Conductive tube 41

[0037] Insulation tube 42

[0038] Positive electrode 5

[0039] Positive electrode lead 51

[0040] Positive electrode lead tube 52

[0041] Positive electrode extension wire 53

[0042] Positive electrode column 54

[0043] Negative electrode 6

[0044] Negative electrode lead 61

[0045] Negative electrode column 62

[0046] Three-way valve 7

[0047] Collimator 8

[0048] Linear drive mechanism 9

[0049] In situ characterization experiment chamber 10 DETAILED DESCRIPTION

[0050] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. In the description of the present invention, it should be noted that the orientation or position relationship indicated by the terms "left side", "right side", "upper side", "lower side", "above", "below", etc. is based on the orientation or position relationship shown in the drawings, which is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0051] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed, detachable, or integral connections; mechanical or electrical connections; direct or indirect connections through an intermediate medium; and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0052] Furthermore, in the description of the present invention, unless otherwise specified, “plurality” means two or more.

[0053] Example 1

[0054] The embodiment of the present invention provides a plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy, see Figure 2 、 Figure 3 and Figure 5 , comprising a micro-leakage valve 1 connected to an external gas generating device and a rear end tube 2, a middle end tube 3 and a front end tube 4 which are nested and connected in sequence along the gas emission direction. The micro-leakage valve 1 is connected and connected to the rear end tube 2. The micro-leakage valve 1 can regulate the amount of gas entering the rear end tube 2 from the gas generating device. The gas coming out of the micro-leakage valve 1 will flow through the rear end tube 2, the middle end tube 3 and the front end tube 4 in sequence. The gas emission direction refers to the flow direction of the gas after it is emitted from the gas generating device. For details, please refer to Figures 2 to 5 The arrows in the middle indicate the direction. Figure 3Also included is a positive electrode lead-out tube 52 arranged across the front-end tube 4 and the middle-end tube 3, the head end of the positive electrode lead-out tube 52 and a part thereof are located in the front-end tube 4, the tail end of the positive electrode lead-out tube 52 penetrates the side wall of the middle-end tube 3, and a positive electrode extension line 53 is arranged in the positive electrode lead-out tube 52, the concepts of the head end and the tail end are both in the direction of gas emission, the gas inlet end is collectively referred to as the tail end, and the gas outlet end is collectively referred to as the head end. Figure 2 Also included are a positive electrode 5, a positive electrode lead 51 led out by the positive electrode 5, a negative electrode 6, and a negative electrode lead 61 led out by the negative electrode 6, the positive electrode lead 51 is connected with the positive electrode extension line 53 and makes it conductive, the negative electrode lead 61 is connected with the front-end tube 4 and makes it conductive, the positive electrode 5 serves to provide a positive voltage, the negative electrode 6 serves to provide a negative voltage, the positive electrode extension line 53 will be conducted when the positive electrode 5 is powered on, and the front-end tube 4 will be conducted when the negative electrode 6 is powered on, because a part of the positive electrode lead-out tube 52 is located in the front-end tube 4, and the positive electrode extension line 53 is located in the positive electrode lead-out tube 52, therefore, when the positive electrode extension line 53 and the front-end tube 4 are powered on, an ionization region will be formed between the positive electrode extension line 53 and the front-end tube 4, the ionization region can be seen in the dashed rectangle in Figure 4 The gas passing through the ionization region will be ionized into plasma. The plasma jet device compatible with near-normal-pressure photoelectron spectroscopy provided by the present application can realize the synchronization of gas delivery and plasma generation at the same position, ensure the uniformity of the plasma entering the chamber 10 for in-situ characterization experiments, and concentrate the plasma in the test area, so as to increase the plasma concentration on the surface of the sample and improve the surface reaction of the sample.

[0055] As a supplementary explanation, the length of the positive electrode lead-out tube 52 is 110-130 mm, preferably 20 mm, the inner diameter is 1-2 mm, preferably 1 mm, and the outer diameter is 2-3 mm, preferably 2 mm; and / or the length of the positive electrode extension line 53 is 115-135 mm, preferably 125 mm, and the diameter is 1-2 mm, preferably 1 mm; and / or the length of the front end tube 4 is 90-110 mm, preferably 100 mm, the inner diameter is 5-7 mm, preferably 6 mm, and the outer diameter is 7-9 mm, preferably 8 mm; and / or the length of the middle end tube 3 is 10~30mm, preferably 20mm, the inner diameter is 2~4mm, preferably 3mm, the outer diameter is 3~5mm, preferably 4mm; and / or, the length of the rear end tube 2 is 550~570mm, preferably 560mm, the inner diameter is 3~5mm, preferably 4mm, the outer diameter is 5.35~7.35mm, preferably 6.35mm; and / or, the material of the positive electrode extension wire 53 is preferably tungsten wire; and / or, the materials of the front end tube 4, the middle end tube 3 and the rear end tube 2 are preferably ceramic; and / or, the material of the positive electrode lead 51 and the negative electrode lead 61 is preferably copper.

[0056] In the plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy provided in the embodiment of the present invention, refer to Figure 3 and Figure 4 The front end tube 4 is provided with a conductive tube 41 and an insulating tube 42 in sequence from the outside to the inside. The insulating tube 42 is nested outside the middle end tube 3. The conductive tube 41 is provided with a negative electrode column 62. The negative electrode lead 61 is connected to the negative electrode column 62 and makes it conductive. The positive electrode lead 52 is also provided with a positive electrode column 54 connected to the positive electrode extension line 53. The positive electrode lead 51 is connected to the positive electrode column 54 and makes it conductive. In a specific embodiment, refer to Figure 3 The ends of the insulating tube 42, the conductive tube 41, and the front end tube 4 are stepped. Specifically, the end portion of the insulating tube 42 is located outside the conductive tube 41, and the end portion of the conductive tube 41 is located outside the front end tube 4. In another specific embodiment, a portion of the positive electrode column 54 is located within the positive electrode lead tube 52 and connected to the positive electrode extension wire 53, while another portion passes through the end of the positive electrode lead tube 52 and is located outside the positive electrode lead tube 52. The positive electrode lead wire 51 is connected to the positive electrode column 54 located outside the positive electrode lead tube 52.

[0057] See Figure 4 In some embodiments, the head of the positive electrode extension wire 53 extends to the outside of the head end of the positive electrode lead-out tube 52. In some embodiments, the head end of the front end tube 4 extends to the outside of the head end of the conductive tube 41. In some embodiments, the head end of the conductive tube 41 extends to the outside of the head end of the insulating tube 42. In one specific implementation, seeFigure 4 , the head end of the insulating tube 42, the head end of the conductive tube 41 and the head end of the front end tube 4 are in a stepped shape, which is explained in detail as follows: the head end portion of the front end tube 4 is located outside the conductive tube 41, and the head end portion of the conductive tube 41 is located outside the insulating tube 42, thereby forming a stepped shape. Furthermore, the length of the head of the front end tube 4 extending to the outside of the conductive tube 41 is 4 to 6 mm, preferably 5 mm; the length of the head end of the conductive tube 41 extending to the outside of the insulating tube 42 is 3 to 5 mm, preferably 4 mm; the length of the head end of the positive electrode extension line 53 extending to the outside of the positive electrode lead-out tube 52 is 4 to 6 mm, preferably 5 mm. In a preferred embodiment, refer to Figure 4 The head end of the conductive tube 41 is flush with the head end of the positive electrode extension line 53. When this embodiment is in use, the positive electrode 5 connects the positive electrode column 54 and the positive electrode extension line 53 through the positive electrode lead 51, and the negative electrode 6 connects the conductive tube 41. The positive electrode lead-out tube 52 is usually made of an insulating material. Only the head end and part of the positive electrode extension line 53 located outside the positive electrode lead-out tube 52 can produce an ionization effect. The insulating tube 42 is also usually made of an insulating material. Only the head end and part of the conductive tube 41 located outside the insulating tube 42 can produce an ionization effect. Therefore, the head end and part of the conductive tube 41 and the head end and part of the positive electrode extension line 53 form an ionization area. The ionization area can be seen in detail. Figure 4 In the dotted rectangular box, when the gas passes through the ionization region in the front tube 4, the gas will be ionized into plasma. As a supplementary explanation, see Figure 1 The positive electrode lead-out tube 52 can usually be set at the position of the center axis of the front end tube 4, so that the cross-section of the ionization area is a uniform ring shape, which can prevent the unevenness of gas ionization caused by different electric field strengths.

[0058] As a supplementary explanation, the material of the positive electrode column 54 is preferably tungsten; and / or, the material of the negative electrode column 62 is preferably stainless steel; and / or, the material of the conductive tube 41 is preferably stainless steel; and / or, the material of the insulating tube 42 is preferably ceramic.

[0059] In the plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy provided in the embodiment of the present invention, refer to Figure 5 and Figure 5The three-way valve 7 is connected with the collimator 8 and the micro leak valve 1 at opposite ends, and the positive electrode lead 51 and the negative electrode lead 61 pass through the three-way valve 7, the collimator 8 and the linear driving mechanism 9 in sequence. The linear driving mechanism 9 is adapted to be connected with the side wall of the in-situ characterization experiment chamber 10, and is usually connected with the side wall of the in-situ characterization experiment chamber 10 by a flange. The side wall is also provided with a corresponding opening, so that the rear-end tube 2 can pass through the side wall of the in-situ characterization experiment chamber 10 and enter the in-situ characterization experiment chamber 10. In the plasma jet device provided by the application, referring to Figure 6 The three-way valve 7, the collimator 8 and the linear driving mechanism 9 are usually connected by flanges. The independent end of the three-way valve 7 is provided with an electrode flange, and the positive electrode 5 and the negative electrode 6 are arranged in the electrode flange. The flanges are preferably CF35 type flanges. The collimator 8 adjusts the distance and angle relationship between the flanges at both ends, so that the plasma jet device can be adjusted in the axial distance of ±5 mm and the inclination angle of ±3°. The collimator 8 is usually PA35-T (UHV Design Ltd.). The linear driving mechanism 9 adjusts the stroke of the plasma jet device in the in-situ photoelectron spectroscopy characterization chamber. The stroke of the linear driving mechanism 9 is usually 90-110 mm, and preferably 100 mm. The linear driving mechanism 9 is usually LSM38-100-H (UHV Design Ltd.).

[0060] The application also provides a use method of the plasma jet device compatible with the near-normal-pressure photoelectron spectroscopy, which at least includes the following steps:

[0061] 1) After the gas passes through the micro leak valve 1, the gas enters the rear-end tube 2, the middle-end tube 3 and the front-end tube 4 in sequence.

[0062] 2) The positive electrode 5 and the negative electrode 6 are powered on, so that the positive electrode extension line 53 connected with the positive electrode lead 51 and the front-end tube 4 connected with the negative electrode lead 61 are in a conductive state. In a specific embodiment, the positive electrode 5 is powered on by the positive electrode lead 51 to make the positive electrode column 54 and the positive electrode extension line 53 conductive. The negative electrode 6 is powered on by the negative electrode column 62 to make the conductive tube 41 conductive. The head of the positive electrode extension line 53 and part thereof and the head of the conductive tube 41 and part thereof form an ionization region.

[0063] 3) The gas is ionized into plasma by the positive electrode extension 53 and the front tube 4 as it passes through the front tube 4. In one embodiment, the gas is ionized into plasma as it passes through the ionization region.

[0064] Embodiment two

[0065] The embodiments of the present application also provide an in-situ photoelectron spectroscopy characterization device, referring to ​ , comprising the plasma jet device compatible with the near-normal-pressure photoelectron spectroscopy as described in embodiment one, further comprising an in-situ characterization experiment chamber 10, the in-situ characterization experiment chamber 10 is suitable for placing a sample, and the plasma jet device is arranged in the side wall of the in-situ characterization experiment chamber 10 and the head end of the front tube 4 is close to the sample. In one embodiment, the linear drive mechanism 9 is installed on the side wall of the in-situ characterization experiment chamber 10, and the corresponding openings are arranged on the part of the side wall, so that the part of the rear tube 2, the middle tube 3 and the front tube 4 can be located in the in-situ characterization experiment chamber 10. The specific principle of the in-situ characterization experiment device can be referred to the patent , application number: 2024221786117. When the linear drive mechanism 9 is used, it can shorten or lengthen itself. Taking the case that the linear drive mechanism 9 gradually lengthens itself as an example: when the linear drive mechanism 9 gradually lengthens itself, it will gradually push away the collimator 8, the three-way valve 7 and the micro-leak valve 1 connected with it in sequence from the in-situ characterization experiment chamber 10, when the micro-leak valve 1 is pushed away from the in-situ characterization experiment chamber 10, the rear tube 2, the middle tube 3 and the front tube 4 connected with the micro-leak valve 1 in sequence will gradually move away from the in-situ characterization experiment chamber 10, and the front tube 4 will gradually move away from the sample. Similarly, when the linear drive mechanism 9 gradually shortens itself, the front tube 4 will gradually move close to the sample. Therefore, the linear drive mechanism 9 can control the sample inlet distance.

[0066] The above only describes the preferred embodiments of the present application, and it should be pointed out that for ordinary skilled in the art, without departing from the technical principles of the present application, a number of improvements and replacements can be made, and these improvements and replacements should also be considered as the protection scope of the present application.

Claims

1. A plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy, characterized by: It comprises a micro-leakage valve (1) connected to an external gas generating device, and a rear end tube (2), a middle end tube (3), and a front end tube (4) which are nested, connected, and communicated in sequence along the gas emission direction, wherein the micro-leakage valve (1) is connected and communicated with the rear end tube (2); It also includes a positive electrode lead-out tube (52) that spans the front end tube (4) and the middle end tube (3), wherein the head end and part of the positive electrode lead-out tube (52) are located in the front end tube (4), and the end of the positive electrode lead-out tube (52) passes through the side wall of the middle end tube (3); a positive electrode extension line (53) is provided in the positive electrode lead-out tube (52); It also includes a positive electrode (5), a positive electrode lead (51) extending from the positive electrode (5), a negative electrode (6), and a negative electrode lead (61) extending from the negative electrode (6); the positive electrode lead (51) is connected to the positive electrode extension line (53) and is electrically conductive thereto, and the negative electrode lead (61) is connected to the front end tube (4) and is electrically conductive thereto; The front end tube (4) is provided with a conductive tube (41) and an insulating tube (42) in sequence from the outside to the inside, and the insulating tube (42) is nested outside the middle end tube (3); the conductive tube (41) is provided with a negative electrode column (62), and the negative electrode lead (61) is connected to the negative electrode column (62) and makes it conductive; the positive electrode lead tube (52) is also provided with a positive electrode column (54) connected to the positive electrode extension line (53), and the positive electrode lead (51) is connected to the positive electrode column (54) and makes it conductive; It also includes one or more of the following technical features: Technical Features 1) The head of the positive electrode extension wire (53) extends outside the head end of the positive electrode lead-out tube (52); Technical feature 2) the head end of the front end tube (4) extends outside the head end of the conductive tube (41); Technical feature 3) The head end of the conductive tube (41) extends outside the head end of the insulating tube (42).

2. The plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy according to claim 1, characterized in that: The positive electrode lead-out tube (52) has a length of 110-130 mm, an inner diameter of 1-2 mm, and an outer diameter of 2-3 mm; and / or, the positive electrode extension wire (53) has a length of 115-135 mm and a diameter of 1-2 mm; And / or, the front end tube (4) has a length of 90-110 mm, an inner diameter of 5-7 mm, and an outer diameter of 7-9 mm; And / or, the middle end tube (3) has a length of 10-30 mm, an inner diameter of 2-4 mm, and an outer diameter of 3-5 mm; And / or, the rear end tube (2) has a length of 550-570 mm, an inner diameter of 3-5 mm, and an outer diameter of 5.35-7.35 mm.

3. The plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy according to claim 1, characterized in that: The conductive tube (41) has a length of 90-110 mm, an inner diameter of 4-6 mm, and an outer diameter of 5-7 mm; and / or the insulating tube (42) has a length of 86-106 mm, an inner diameter of 3-5 mm, and an outer diameter of 4-6 mm; and / or the negative electrode column (62) has a length of 2-4 mm and a diameter of 1-2 mm; and / or the positive electrode column (54) has a length of 2-4 mm and a diameter of 1-2 mm.

4. The plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy according to claim 1, characterized in that: Include one or more of the following technical features: If the technical feature 1) is included, the length of the head of the positive electrode extension line (53) extending outward is 4 to 6 mm; If technical feature 2) is included, the outward extension length of the head end of the front end tube (4) is 4 to 6 mm; If technical feature 3) is included, the length of the outward extension of the head end of the conductive tube (41) is 3 to 5 mm.

5. The plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy according to claim 1, characterized in that: The invention also includes a three-way valve (7), a collimator (8) and a linear drive mechanism (9) which are sequentially connected along the gas emission direction and are all located outside the rear end tube (2); the opposite ends of the three-way valve (7) are respectively connected to the collimator (8) and the micro-leak valve (1); the positive electrode lead (51) and the negative electrode lead (61) sequentially pass through the three-way valve (7), the collimator (8) and the linear drive mechanism (9); the linear drive mechanism (9) is suitable for connecting to the side wall of the chamber (10) for in-situ characterization experiments.

6. The plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy according to claim 5, characterized in that: An electrode flange is provided on an independent end of the three-way valve (7), and the positive electrode (5) and the negative electrode (6) are both provided in the electrode flange; and / or, the axial angle of the collimator (8) is adjusted to ±5 mm, and the tilt angle is adjusted to ±3°; And / or, the stroke of the linear drive mechanism (9) is 90-110 mm.

7. A method for using the plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy according to any one of claims 1 to 6, characterized in that: It includes at least the following steps: After passing through the micro-leak valve (1), the gas enters the rear end tube (2), the middle end tube (3) and the front end tube (4) in sequence; The positive electrode (5) and the negative electrode (6) are energized, so that the positive electrode extension wire (53) connected to the positive electrode lead (51) and the front end tube (4) connected to the negative electrode lead (61) are in a conductive state; When the gas passes through the front end tube (4), it is ionized into plasma by the positive electrode extension wire (53) and the front end tube (4).

8. An in-situ photoelectron spectroscopy characterization device, characterized by: The invention comprises a plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy as claimed in any one of claims 1 to 6, and further comprises an in-situ characterization experiment chamber (10), wherein the in-situ characterization experiment chamber (10) is suitable for placing a sample, and the plasma spray gun device is arranged in the side wall of the in-situ characterization experiment chamber (10) and the head end of the front end tube (4) is close to the sample.

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