Plasma torch device compatible with near-normal-pressure photoelectron spectroscopy
By designing a plasma spray gun device compatible with nearly normal -voltage light electronics spectrum, the synchronization of gas conversion and plasma is achieved, solving the problem of low concentration of medium ion body in existing technology and the generation of by -products. The accuracy of nature and research results.
Patent Information
- Application Number
- CN202411469928.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-21
- Publication Date
- 2025-01-21
- Estimated Expiration
- 2044-10-21
AI Technical Summary
The prior art is difficult to effectively generate plasma in the sample surface area, resulting in a low plasma concentration, a lack of obvious reaction on the sample surface, and the plasma is prone to react with adsorbents on the chamber wall to produce by-products, affecting the research results.
Design a plasma spray gun device that is compatible with near-normal pressure photoelectron spectroscopy. Through micro-leak valves and nested-connected pipeline structures, gas transportation and plasma generation are synchronized to ensure plasma uniformity and concentration and improve sample quality. Surface plasma concentration.
The uniform and centralized distribution of the plasma on the surface area of the sample is realized, which improves the significant response of the sample surface reaction, reduces the generation of by -products, and improves the accuracy of the research results.
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Figure CN119342673A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of in-situ spectroscopy characterization, in particular to a plasma spray gun device compatible with near-normal pressure photoelectron spectroscopy. Background Art
[0002] Plasma is the fourth state of matter besides solid, liquid and gas. The large number of ions, high-energy electrons and excited atomic molecules in it can provide active groups that are easy to react chemically, making the plasma-enhanced chemical transformation process show unconventional behavior under special external fields. It is one of the cutting-edge development directions that has attracted global attention and is widely used in many fields such as energy, environment, materials, and chemical engineering. Near-normal pressure photoelectron spectroscopy is crucial in scientific research. It can observe and record reactions and material changes in actual environments. Its elemental and chemical specificity, high surface sensitivity and ease of use are helpful for in-depth research on the electronic geometry of materials, the atomic structure of the coordination environment and morphological changes, and to explore the dynamic changes of the sample surface during the reaction. This has greatly promoted the development of new materials, new catalysts and new drugs, and is widely used in chemistry, materials science, biology and other fields.
[0003] Plasma is a typical multidisciplinary field, and research is still relatively scarce. Near-ambient pressure photoelectron spectroscopy can characterize the chemical state and electronic structure of the material surface in situ. It is widely used in catalytic reactions and semiconductor technology related 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 research uses non-in-situ or quasi-in-situ methods (for example, by treating the sample in a plasma environment and then transferring it to a test chamber for vacuum characterization) that cannot change the high vacuum environment during the characterization process. Although it helps to understand plasma-induced surface phenomena, it does not have the ability to perform in-situ characterization of the changes in the surface chemical state and electronic structure of the sample in a plasma environment. This information is the key to revealing the mechanism of interaction 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), the gas is transported into the chamber through a micro-leak valve 1, and a voltage is applied to the electrodes in the chamber through 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 through an electron energy analyzer, thereby obtaining information on the chemical state and electronic structure of the material surface.
[0006] However, the area where plasma is generated is far from the test area on the sample surface, the plasma concentration in the test area is low, the sample surface reaction is not obvious, and the plasma will react with the adsorbent on the chamber wall to produce many by-products, which will change the sample surface results and affect the research results. Therefore, designing a new plasma generation device suitable for in-situ photoelectron spectroscopy characterization is of great significance to the entire plasma in-situ characterization technology.
[0007] Given the importance of plasma in-situ characterization technology to the development of materials science and the importance of how to generate plasma to plasma in-situ characterization technology, how to effectively generate plasma in the sample surface area and perform in-situ characterization is a key technical issue that needs to be solved urgently, which will have a huge impact on further promoting the development of materials science. Summary of the invention
[0008] In order to solve the above problems, the first aspect of the present invention provides a plasma spray gun device compatible with near-atmospheric pressure photoelectron spectroscopy, which can realize the synchronous delivery of gas and generation of plasma at the same position, ensure the uniformity of plasma entering the chamber for in-situ characterization experiments, and concentrate the plasma in the test area, so as to increase the plasma concentration on the sample surface and enhance the surface reaction of the sample.
[0009] The first aspect of the present invention provides a plasma spray gun device compatible with near-normal pressure photoelectron energy spectrum, comprising a micro-leakage valve of an external gas generating device and a rear end tube, a middle end tube and a front end tube which are nested, connected and connected in sequence along the gas emission direction, wherein the micro-leakage valve is connected and connected to the rear end tube; further comprising a positive electrode lead-out tube which is arranged across the front end tube and the middle end tube, wherein the head end and part of the positive electrode lead-out tube are located in the front end tube, and the end of the positive electrode lead-out tube passes through the side wall of the middle end tube; a positive electrode extension line is arranged in the positive electrode lead-out tube; further comprising a positive electrode, a positive electrode lead wire led from the positive electrode, a negative electrode and a negative electrode lead wire led from the negative electrode; the positive electrode lead wire is connected to the positive electrode extension line and makes it conductive, and the negative electrode lead wire is connected to the front end tube and makes it conductive.
[0010] In some feasible embodiments, the positive electrode lead-out tube 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 line has a length of 115-135 mm, and a diameter of 1-2 mm; and / or the front end tube 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 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 has a length of 550-570 mm, an inner diameter of 3-5 mm, and an outer diameter of 5.35-7.35 mm.
[0011] In a feasible embodiment, a conductive tube and an insulating tube are sequentially provided inside the front end tube from the outside to the inside, and the insulating tube is nested outside the middle end tube; a negative electrode column is provided on the conductive tube, and the negative electrode lead is connected to the negative electrode column to make it conductive; a positive electrode column connected to the positive electrode extension line is also provided in the positive electrode lead tube, and the positive electrode lead is connected to the positive electrode column to make it conductive.
[0012] In some feasible embodiments, the conductive tube has a length of 90 to 110 mm, an inner diameter of 4 to 6 mm, and an outer diameter of 5 to 7 mm; and / or, the insulating tube has a length of 86 to 106 mm, an inner diameter of 3 to 5 mm, and an outer diameter of 4 to 6 mm; and / or, the negative electrode column has a length of 2 to 4 mm, and a diameter of 1 to 2 mm; and / or, the positive electrode column has a length of 2 to 4 mm, and a diameter of 1 to 2 mm.
[0013] In some feasible embodiments, one or more of the following technical features are included: 1) the head of the positive electrode extension wire 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 feasible embodiments, one or more of the following technical features are included: if the technical feature 1) in the above embodiment is included, the length of the head of the positive electrode extension wire extending outward is 4 to 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 to 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 to 5 mm.
[0015] In a feasible embodiment, it also includes a three-way valve, a collimator and a linear drive mechanism which are connected in sequence along the gas emission direction and are all located outside the rear end tube; the opposite ends of the three-way valve are respectively connected to the collimator and the micro-leak valve, 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 suitable for connecting to the side wall of the chamber for in-situ characterization experiments.
[0016] In some feasible embodiments, an electrode flange is provided on an independent end of the three-way valve, and the positive electrode and the negative electrode are both provided in the electrode flange; and / or, the axial angle of the collimator is adjusted to ±5 mm, and the tilt angle is adjusted to ±3°; and / or, the stroke of the linear drive mechanism is 90 to 110 mm.
[0017] The present invention also provides a method for using a plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy, which comprises at least the following steps:
[0018] 1) After passing through the micro-leak valve, the gas enters the rear end pipe, the middle end pipe and the front end pipe in sequence;
[0019] 2) The positive electrode and the negative electrode are energized so that the positive electrode extension wire connected to the positive electrode lead and the front end tube connected to the negative electrode lead are in a conductive state;
[0020] 3) When the gas passes through the front end tube, it is ionized into plasma by the positive electrode extension wire and the front end tube.
[0021] The second aspect of the present invention provides an in-situ photoelectron energy spectrum characterization device, including a plasma spray gun device compatible with near-atmospheric pressure photoelectron energy spectrum as provided in the first aspect of the present invention, characterized in that it also includes an in-situ characterization experiment chamber, the in-situ characterization experiment chamber is suitable for placing samples, the plasma spray gun device is penetrated 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 present invention provides a plasma spray gun device and an in-situ photoelectron spectroscopy characterization device compatible with near-normal pressure photoelectron spectroscopy, which have the following beneficial effects:
[0023] 1) The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy provided by the present invention can realize the synchronous delivery of gas and generation of plasma at the same position, thereby ensuring the uniformity of the plasma entering the chamber for in-situ characterization experiments, and can concentrate the plasma in the test area, thereby increasing the plasma concentration on the sample surface and enhancing the surface reaction of the sample.
[0024] 2) The collimator and linear drive mechanism in the plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy provided by the present invention can rotate or retract the plasma spray gun part located in the chamber for characterization experiments, thereby achieving the regulation of the distance and angle between the plasma and the sample. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 It is a sample injection device in the prior art.
[0026] Figure 2 The figure is a schematic diagram of the overall structure of a plasma spray gun device compatible with near-normal pressure photoelectron spectroscopy according to the present invention.
[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 invention.
[0028] Figure 4 It is a cross-sectional view of the front end tube, conductive tube, insulating tube, positive electrode lead-out tube and ionization region of the present invention.
[0029] Figure 5 It is a cross-sectional view of the three-way valve, collimator and linear drive mechanism of the present invention.
[0030] Figure 6 The figure is a schematic diagram of the overall structure of an in-situ photoelectron energy spectrum 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 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 the field without creative work belong to 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" and the like 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 used for descriptive purposes only 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 clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0052] Furthermore, in the description of the present invention, unless otherwise specified, “plurality” means two or more.
[0053] Embodiment 1
[0054] The embodiment of the present invention provides a plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy, referring to 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 Figure 2 to Figure 5 The arrows in the figure indicate the direction. Figure 3, and also includes a positive electrode lead-out tube 52 that spans the front end tube 4 and the middle end tube 3. 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. The concepts of head end and end end are based on the gas emission direction. The gas inlet end is collectively referred to as the end end, and the gas outlet end is collectively referred to as the head end. Continue to read Figure 2 , further comprising a positive electrode 5, a positive electrode lead 51 derived from the positive electrode 5, a negative electrode 6 and a negative electrode lead 61 derived from the negative electrode 6, the positive electrode lead 51 being connected to the positive electrode extension line 53 and making it conductive, the negative electrode lead 61 being connected to the front end tube 4 and making it conductive, the positive electrode 5 is used to provide a positive electrode voltage, and the negative electrode 6 is used to provide a negative electrode voltage, when the positive electrode 5 is energized, the positive electrode extension line 53 will be conductive, and when the negative electrode 6 is energized, the front end tube 4 will be conductive, because a portion 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 energized, an ionization region will be formed between the positive electrode extension line 53 and the front end tube 4, and the ionization region can be seen in detail Figure 4 The dotted rectangular frame in the figure shows that the gas passing through the ionization area will be ionized into plasma. The plasma spray gun device compatible with near-normal pressure photoelectron spectroscopy provided by the present invention can realize the simultaneous delivery of gas and generation of plasma at the same position, thereby ensuring the uniformity of the plasma entering the chamber 10 for in-situ characterization experiments, and can concentrate the plasma in the test area, thereby increasing the plasma concentration on the sample surface and improving 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-ambient 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, 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 to make 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 to make it conductive. In a specific embodiment, refer to Figure 3 , the end of the insulating tube 42, the end of the conductive tube 41 and the end of the front end tube 4 are stepped, which is explained in detail as follows: 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 in the positive electrode lead-out tube 52 and connected to the positive electrode extension line 53, and the other portion passes through the end of the positive electrode lead-out tube 52 and is located outside the positive electrode lead-out tube 52, and the positive electrode lead 51 is connected to the positive electrode column 54 located outside the positive electrode lead-out tube 52.
[0057] See also Figure 4 In some embodiments, the head of the positive electrode extension line 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 a specific implementation, refer to Figure 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 wire 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 the present embodiment is in use, the positive electrode 5 makes the positive electrode column 54 and the positive electrode extension line 53 conductive through the positive electrode lead 51, and the negative electrode 6 makes the conductive tube 41 conductive. The positive electrode lead-out tube 52 is usually made of insulating material, and only the head end and part of the positive electrode extension line 53 outside the positive electrode lead-out tube 52 can produce ionization. The insulating tube 42 is also usually made of insulating material, and only the head end and part of the conductive tube 41 outside the insulating tube 42 can produce ionization. Therefore, the head end and part of the conductive tube 41 and the head 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 dashed rectangular box in the figure, when the gas passes through the ionization region in the front tube 4, the gas will be ionized into plasma. Figure 4 The positive electrode lead-out tube 52 can usually be arranged at the position of the center axis of the front end tube 4, so that the cross-sectional shape of the ionization region 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-ambient pressure photoelectron spectroscopy provided in the embodiment of the present invention, refer to Figure 1 and Figure 5, 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, and 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, which is explained as follows: the positive electrode lead 51 and the negative electrode lead 61 pass through an independent end of the three-way valve 7, pass out from the end of the three-way valve 7 connected to the collimator 8 and sequentially pass through the collimator 8 and the linear drive mechanism 9. The linear drive mechanism 9 is suitable for connecting to the side wall of the in-situ characterization experiment chamber 10. Usually, the linear drive mechanism 9 is connected to the side wall of the in-situ characterization experiment chamber 10 by a flange, and this part of 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 spray gun device provided by the present invention, refer to Figure 5 , the three-way valve 7, the collimator 8 and the linear drive mechanism 9 are usually connected by flanges. 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. The above flanges are preferably flanges of model CF35. The function of the collimator 8 is to adjust the distance and angle relationship between the flanges at both ends of itself, so that the plasma spray gun device described in the present invention can have an axial distance adjustment of ±5mm and an inclination angle adjustment of ±3°. The model of the collimator 8 is usually PA35-T (UHV Design Ltd.). The function of the linear drive mechanism 9 is to adjust the stroke of the plasma spray gun device described in the present invention in the in-situ photoelectron energy spectrum characterization chamber. The stroke of the linear drive mechanism 9 is usually 90 to 110mm, preferably 100mm, and the model of the linear drive mechanism 9 is usually LSM38-100-H (UHV Design Ltd.).
[0060] The embodiment of the present invention further provides a method for using a plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy, comprising at least the following steps:
[0061] 1) After passing through the micro-leakage valve 1, the gas enters the rear end pipe 2, the middle end pipe 3 and the front end pipe 4 in sequence.
[0062] 2) 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 wire 51 and the front end tube 4 connected to the negative electrode lead wire 61 are in a conductive state. In a specific embodiment, the positive electrode 5 connects the positive electrode column 54 and the positive electrode extension wire 53 through the positive electrode lead wire 51, and the negative electrode 6 connects the conductive tube 41 through the negative electrode column 62, and an ionization area is formed between the head and part of the positive electrode extension wire 53 and the head end and part of the conductive tube 41.
[0063] 3) 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. In a specific embodiment, when the gas passes through the ionization region, it is ionized into plasma.
[0064] Embodiment 2
[0065] The present invention also provides an in-situ photoelectron spectroscopy characterization device, see Figure 6 , including the plasma spray gun device compatible with near-normal pressure photoelectron spectroscopy as described in Example 1, and also including an in-situ characterization experiment chamber 10, wherein the in-situ characterization experiment chamber 10 is suitable for placing samples, 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. In a specific embodiment, the linear drive mechanism 9 is installed on the side wall of the in-situ characterization experiment chamber 10, and the side wall is provided with corresponding openings so that part of the rear end tube 2, the middle end tube 3 and the front end 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 found in the patent , application number: 2024221786117. When the linear drive mechanism 9 is in use, it can shorten or lengthen itself. For example, when it gradually lengthens itself, when the linear drive mechanism 9 gradually lengthens, the collimator 8, the three-way valve 7 and the micro-leakage valve 1 connected thereto in sequence will be gradually pushed away from the in-situ characterization experiment chamber 10. When the micro-leakage valve 1 is pushed away from the in-situ characterization experiment chamber 10, the rear end tube 2, the middle end tube 3 and the front end tube 4 connected thereto in sequence will gradually move toward the outside of the in-situ characterization experiment chamber 10, and the front end tube 4 will gradually move away from the sample. Similarly, when the linear drive mechanism 9 gradually shortens, the front end tube 4 will gradually approach the sample. Therefore, the control of the injection distance can be achieved through the linear drive mechanism 9.
[0066] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and substitutions can be made without departing from the technical principles of the present invention. These improvements and substitutions should also be regarded as the scope of protection of the present invention.
Claims
1. A plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy, characterized in that: It comprises a micro-leakage valve (1) connected to an external gas generating device, and a rear end pipe (2), a middle end pipe (3) and a front end pipe (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 pipe (2); It also includes a positive electrode lead-out tube (52) which is arranged across 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); and a positive electrode extension line (53) is arranged in the positive electrode lead-out tube (52); It also includes a positive electrode (5), a positive electrode lead (51) derived from the positive electrode (5), a negative electrode (6), and a negative electrode lead (61) derived from the negative electrode (6); the positive electrode lead (51) is connected to a positive electrode extension line (53) to make it conductive, and the negative electrode lead (61) is connected to a front end tube (4) to make it conductive.
2. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 1, characterized in that: The positive electrode lead-out tube (52) has a length of 110 to 130 mm, an inner diameter of 1 to 2 mm, and an outer diameter of 2 to 3 mm; and / or, the positive electrode extension wire (53) has a length of 115 to 135 mm and a diameter of 1 to 2 mm; And / or, the front end tube (4) has a length of 90 to 110 mm, an inner diameter of 5 to 7 mm, and an outer diameter of 7 to 9 mm; And / or, the length of the middle end tube (3) is 10 to 30 mm, the inner diameter is 2 to 4 mm, and the outer diameter is 3 to 5 mm; And / or, the length of the rear end tube (2) is 550-570 mm, the inner diameter is 3-5 mm, and the outer diameter is 5.35-7.35 mm.
3. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 1 or 2, characterized in that: 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) to make 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) to make it conductive.
4. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 3, characterized in that: The conductive tube (41) has a length of 90 to 110 mm, an inner diameter of 4 to 6 mm, and an outer diameter of 5 to 7 mm; and / or, the insulating tube (42) has a length of 86 to 106 mm, an inner diameter of 3 to 5 mm, and an outer diameter of 4 to 6 mm; and / or, the negative electrode column (62) has a length of 2 to 4 mm, and a diameter of 1 to 2 mm; and / or, the positive electrode column (54) has a length of 2 to 4 mm, and a diameter of 1 to 2 mm.
5. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 3, characterized in that: Includes one or more of the following technical features: 1) The head of the positive electrode extension wire (53) extends toward the outside of the head end of the positive electrode lead-out tube (52); 2) The head end of the front end tube (4) extends toward the outside of the head end of the conductive tube (41); 3) The head end of the conductive tube (41) extends outside the head end of the insulating tube (42).
6. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 5, characterized in that: Includes 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 length of the head end of the front end tube (4) extending outward is 4 to 6 mm; If technical feature 3) is included, the length of the head end of the conductive tube (41) extending outward is 3 to 5 mm.
7. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 1, characterized in that: The invention also comprises a three-way valve (7), a collimator (8) and a linear drive mechanism (9) which are connected in sequence 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) pass through the three-way valve (7), the collimator (8) and the linear drive mechanism (9) in sequence; and the linear drive mechanism (9) is suitable for being connected to the side wall of a chamber (10) for in-situ characterization experiments.
8. The plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to claim 7, 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 to 110 mm.
9. A method for using the plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy according to any one of claims 1 to 8, characterized in that: At least the following steps are included: 1) 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; 2) 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 wire (51) and the front end tube (4) connected to the negative electrode lead wire (61) are in a conductive state; 3) 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).
10. An in-situ photoelectron spectroscopy characterization device, characterized in that: The invention comprises a plasma spray gun device compatible with near-ambient pressure photoelectron spectroscopy as claimed in any one of claims 1 to 8, and also 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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