A full fluorescence yield detector for in-situ soft x-ray absorption spectroscopy

By employing a large-aperture photomultiplier tube, a double gold mesh structure, and an improved detector design in the soft X-ray fluorescence detector, the problem of severe signal interference in in-situ experiments was solved, achieving efficient fluorescence signal collection and signal purity, making it suitable for synchrotron radiation soft X-ray spectroscopy detection devices.

CN116953004BActive Publication Date: 2026-03-17UNIV OF SCI & TECH OF CHINA
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Patent Information

Application Number
CN202310865508.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-14
Publication Date
2026-03-17
Estimated Expiration
2043-07-14

AI Technical Summary

Technical Problem

Existing soft X-ray fluorescence detectors suffer from severe signal interference in in-situ experiments. In particular, photoelectron and positive ion interference signals have a significant impact on the accuracy and signal-to-noise ratio of fluorescence signals, and the traditional single gold mesh structure cannot effectively shield various interference signals.

Method used

It employs a large-diameter photomultiplier tube, a double gold mesh structure, and an improved detector top angle design. Combined with the fixing method of springs and rubber pads, it uses positive and negative voltages applied to the two layers of gold mesh to shield interference signals. It also adopts a spliced ​​semi-cylindrical design to enhance the signal collection angle and stability.

Benefits of technology

It improves the collection efficiency of fluorescence signals, reduces background noise, and achieves effective shielding of photoelectrons and positive ions, ensuring signal purity and accuracy in complex in-situ environments.

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Abstract

The application provides a full fluorescence yield detector for in-situ soft X-ray absorption spectroscopy, which is based on a photomultiplier and can collect weak fluorescence signals excited by soft X-rays under in-situ conditions (reactions under simulated complex environment conditions). A large-diameter photomultiplier is used and the top angle of the detector is improved to increase the fluorescence collection angle as much as possible to improve the signal strength; double gold meshes are used and different voltages are added to shield interference signals such as photoelectrons and positive ions of non-fluorescence yield at the same time; a spliced half-cylinder barrel design is used to realize shielding and facilitate maintenance and replacement of the photomultiplier; a spring and rubber pad are used in cooperation with a screw to fasten the mode, which can maintain good electrode contact while avoiding overpressure damage to the photomultiplier and can work stably in a vibrating environment. The application optimizes the detector from the aspects of the structure of the detector, detection efficiency, signal interference shielding, maintenance convenience and the like.
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Description

Technical Field

[0001] This invention belongs to the field of synchrotron radiation soft X-ray spectroscopy detection devices, specifically relating to a full-fluorescence yield detector for in-situ soft X-ray absorption spectroscopy. Background Technology

[0002] X-ray absorption spectroscopy is one of the important methods for characterizing the electronic structure of materials. When a sample is irradiated with X-rays, electrons at corresponding energy levels absorb energy and are excited to higher energy levels, while inner-shell orbitals lose electrons to form holes. When excited electrons de-excite or electrons from other energy levels fill the holes, energy is emitted outward in the form of fluorescence or excited Auger electrons. By measuring the emitted fluorescence or electron yield, the absorption intensity of the material to X-rays can be measured, allowing for in-depth studies of the structure-property relationship of the material.

[0003] Soft X-ray absorption spectroscopy commonly uses an energy range of 180–2000 eV, which can cover the 1s energy level of boron, carbon, nitrogen, oxygen, sodium, magnesium, aluminum, and silicon, as well as the 2p energy level of 3d transition metals such as iron, cobalt, nickel, copper, and zinc. It is of great significance for materials science research in fields such as energy science, information storage, catalytic synthesis, biomedicine, and semiconductors.

[0004] The core component for this type of detection is the soft X-ray detector. Because soft X-rays penetrate materials to a relatively short depth, indirect detection modes such as fluorescence yield and electron yield are typically used. However, the fluorescence yield in the soft X-ray band is generally 1 to 3 orders of magnitude lower than the electron yield. Furthermore, in in-situ experiments, the complex sample environment can interfere with signal purity, placing higher demands on the fluorescence detector: it not only needs to filter and amplify the signal but also needs to shield against various electrons and positive ions in the vacuum chamber to improve signal purity.

[0005] Currently, research-grade soft X-ray fluorescence detectors are typically developed based on photosensitive elements such as photomultiplier tubes (PMTs), multiple channel plates (MSPs), photodiodes, silicon drift detectors (SDDs), and charge-coupled devices (CCDs). Among these, PMTs are widely used in soft X-ray fluorescence detection due to their low cost and immunity to visible light interference. Since PMTs respond to electrons, ions, and X-rays, a gold mesh is usually placed in front of the PMT and a bias voltage is applied to shield ions and electrons. However, the polarity and level of the applied voltage remain controversial. For example, the gold mesh is usually close to the sample; applying too high a positive voltage can affect the accuracy of the sample's fluorescence signal, while applying a negative voltage can hinder photoelectrons, leading to a decrease in electron yield and hindering multi-mode signal collection. These effects are particularly pronounced in weak signal collection and multi-physics field measurements, such as in-situ experiments. Therefore, a more rational detector structure needs to be designed to achieve low-interference and high-purity fluorescence signal measurement. Summary of the Invention

[0006] This invention addresses the complex environmental requirements of in-situ experiments by proposing a full-fluorescence yield detector for in-situ soft X-ray absorption spectroscopy. It is a photomultiplier tube-based detector system structure that provides a more efficient method for collecting fluorescence signals in the soft X-ray band. This invention designs a detector based on a photomultiplier tube that can collect weak fluorescence signals excited by soft X-rays under in-situ conditions (simulating reactions under complex environmental conditions). It employs a large-aperture photomultiplier tube and improves the detector's top angle design to maximize the fluorescence collection angle and enhance signal strength. A double gold mesh with varying voltages is used to simultaneously shield non-fluorescent yield interference signals such as photoelectrons and positive ions. A modular semi-cylindrical design achieves shielding while facilitating photomultiplier tube maintenance and replacement. A spring and rubber pad combined with screws for fastening maintains good electrode contact while preventing overvoltage damage to the photomultiplier tube and allows for stable operation in vibrating environments.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] A full-fluorescence yield detector for in-situ X-ray absorption spectroscopy includes an interference signal shielding mesh assembly, a fluorescence signal receiver assembly, a shielding and support assembly, and an electrical connection and external sealing assembly.

[0009] The interference signal shielding mesh assembly comprises an aluminum ring electrode, a gold mesh, an insulating ring, a first high-voltage conductor, an outer insulating sleeve, insulating screws, and hexagonal screws. Two layers of gold mesh are separated by the insulating ring. The voltage on the gold mesh is provided by the first high-voltage conductor fixed to the aluminum ring electrode. The first high-voltage conductor is fastened to the aluminum ring electrode by hexagonal screws. The aluminum ring electrode, gold mesh, and insulating ring form a "sandwich" structure, which is then fastened to the outer insulating sleeve by insulating screws.

[0010] The fluorescence signal receiver assembly includes a photomultiplier tube fixing component, a photomultiplier tube, a rubber pad, first fastening screws, gold-plated screws, washers, a spring, a second high-voltage wire, a signal wire, and a fastening nut. Three first fastening screws are placed on the rubber pad to fix the photomultiplier tube to the fixing component. Two gold-plated screws are connected to the electrodes of the photomultiplier tube. The spring is separated from the lower surface of the photomultiplier tube by the washers. The second high-voltage wire is then connected in series with the gold-plated screws via a gold-plated copper terminal and finally secured with the fastening nut. The output signal of the photomultiplier tube is led out through the signal wire connected in series at the end of the signal terminal, and the signal wire is also secured with the fastening nut. The rubber pad is made of flexible Viton rubber.

[0011] The shielding and support assembly includes a semi-cylindrical outer shell and countersunk screws; the countersunk screws serve as fasteners to connect the semi-cylindrical outer shell, the outer insulating sleeve, the multiplier tube fixing component, and the outer shell connector to support and position the detector as a whole.

[0012] The electrical connection and external sealing assembly is assembled from a high-voltage electrical feeder, a wire connector, a metal sleeve, an insulating support platform, a housing connector, second fastening screws, and a support platform positioning screw. The housing connector is installed on the insulating support platform by four second fastening screws, and then on the high-voltage electrical feeder by the support platform positioning screw. The wire connector mates with the four pins on the high-voltage electrical feeder. The metal sleeve mates with the gap between the pins and the flange face on the high-voltage electrical feeder. The first high-voltage wire, the second high-voltage wire, and the signal wire connected to the first layer of gold mesh pass through the through holes on the insulating support platform and the housing connector and are inserted into the wire connector. The internal hex screws on the side of the wire connector are tightened to fix the four wires.

[0013] Furthermore, the aluminum annular electrode is a hollow ring with a threaded hole; the gold mesh is a mesh with 90% light transmittance; the insulating ring is a hollow ring; the outer insulating sleeve is a hollow conical top cylinder; and the internal hexagonal screw is made of stainless steel.

[0014] Furthermore, the gold mesh material is pure gold, the gold mesh thickness is 20μm, the distance between the two gold mesh layers is 3mm, and the end facing the sample uses a gold mesh with 90% transmittance to filter interference signals, utilizing the chemical stability of gold to cope with the complex acid, alkali and organic environments of in-situ experiments.

[0015] Furthermore, the top cone angle of the outer insulating sleeve is 0° to 90°.

[0016] Furthermore, the photomultiplier tube fixing component is a cylindrical platform with a central stepped surface; the photomultiplier tube has a tapered receiving port; the rubber pad is an L-shaped perforated thin rubber pad; the two ends of the spring are separated by washers and mounted on gold-plated screws; the second high-voltage wire is a wire with an external insulation layer; and the signal line is a double-shielded wire with an external insulation layer.

[0017] Furthermore, the photomultiplier tube is fixed to the photomultiplier tube fixture using a flexible rubber pad and a first fastening screw. This ensures good electrical contact while avoiding damage to the ceramic components caused by sudden changes in hard contact pressure when fixing the photomultiplier tube.

[0018] Furthermore, the gold-plated screw and fastening nut are M1.6, 12mm in length, and made of stainless steel; the spring has a free length of 3.5mm and a diameter of 0.2mm, and is made of stainless steel, high-carbon spring steel, titanium, or a special alloy; the dimensions of the gold-plated screw and spring are adjustable according to the photomultiplier tube hole position and fixing pressure requirements; a ring-shaped metal terminal is used in conjunction with the fastening nut to connect the second high-voltage wire and the gold-plated screw, enabling quick assembly and disassembly.

[0019] Furthermore, the upper part of the high-voltage electrical feeder is provided with a knife-edge flange, and the lower part is provided with four high-voltage electrode pins; the wire connector is a hollow cylinder with a fine groove at the bottom and a threaded hole on the upper side; the metal sleeve is a hollow cylinder with a fine groove; the insulating support platform is a cylinder with a groove at the bottom and a threaded hole and a through hole at the top; the outer shell connector is a cylinder with a hole.

[0020] Furthermore, a Faraday cage is formed by using a stainless steel semi-cylindrical shell, a gold-plated metal sleeve, and aluminum shell connectors to physically and electromagnetically shield external interference signals, ensuring the reliability of the signal during fluorescence reception and gain, and reducing background noise; the semi-cylindrical shell is made of 316L stainless steel, aluminum, or copper.

[0021] Furthermore, the electrical connections of the detector are as follows:

[0022] The flange of the high-voltage electrical feedthrough 4-1 includes interface A, interface B, interface C, and interface D. Interface A is connected to the first layer of gold mesh and is given a positive voltage ranging from 0 to +100V to shield positive ions in the vacuum chamber. Interface B is connected to the second layer of gold mesh and the negative terminal of the photomultiplier tube and is given a negative high voltage ranging from -400 to -2500V. The negative voltage of the second layer of gold mesh is used to shield photoelectrons emitted from the sample, and the negative terminal of the photomultiplier tube is used to form a voltage drop between itself and the positive terminal to amplify the secondary electrons excited by the incident light. Interface C is connected to a 4MΩ resistor R and the negative terminal of the photomultiplier tube, with its external end grounded. Through resistor voltage division, the potential at terminal C is 10 to 100V lower than that at the ground terminal, ensuring that the amplified electrons are drawn towards interface D, which is connected to the signal terminal, under the influence of the electric field, thus improving signal collection efficiency. Interface D is connected to the signal terminal for signal reception and transmission.

[0023] Furthermore, the operating temperature range is from room temperature to 70℃, with a maximum baking temperature of 200℃; the detector mounting flange size is DN40CF, the inner diameter of the vacuum pipe is not less than 38mm, and the cavity vacuum level during operation is better than 1×10⁻⁶. -7 mbar; the number of flange interfaces for high-voltage electrical feedthrough is not less than 4, and the withstand voltage is not less than 3kV; the length from the top of the detector to the flange surface is in the range of 100-400mm, which can be customized according to requirements; according to the characteristics of in-situ experiments, the fluorescence emission range is a cone angle of 70°, while meeting the requirements of a 40mm distance from the sample and a minimum angle of 30° with the incident X-ray, thus meeting the detection requirements of in-situ experiments.

[0024] Furthermore, polyetheretherketone, polyimide, and alumina ceramics are used as insulating materials, or polytetrafluoroethylene, boron nitride, and aluminum nitride ceramics are used as insulating materials.

[0025] Furthermore, non-standard parts can be precision machined using polyetheretherketone (PEEK) or stainless steel, or titanium alloys, aluminum, copper, polyimide, mica, or ceramics can be used as machinable materials with the required mechanical strength, depending on the application environment.

[0026] Furthermore, the gold mesh can be replaced with copper, nickel, or stainless steel, and the thickness of a single layer and the distance between two layers of metal mesh can be adjusted as needed.

[0027] Furthermore, the top cone angle of the outer insulating sleeve is 30°.

[0028] Furthermore, the semi-cylindrical shell is replaced with a semi-prismatic shell to form a Faraday cage and provide support.

[0029] Beneficial effects:

[0030] This invention mainly optimizes the detector's structure, detection efficiency, signal interference shielding, and maintenance convenience, with specific beneficial effects including:

[0031] (1) The present invention optimizes the spatial structure and fixing method of the detector and adopts a compact design, such as ring electrodes, to reduce the space required for fixing components. Thus, within a limited space, a 20mm diameter photomultiplier tube can replace the previous 10mm diameter photomultiplier tube, and the signal acceptance angle is increased to four times the original, which helps to collect weak fluorescence signals in in-situ experiments.

[0032] (2) In in-situ experiments, the experimental environment is complex. When X-rays irradiate the sample, various ionized positive ions and excited photoelectrons are generated. Without shielding, these interference signals will significantly affect the accuracy and signal-to-noise ratio of the collected fluorescence signals. This invention uses a Faraday cage with physical isolation to shield the interference signals. The photomultiplier tube, high-voltage wires, signal lines, and electrical interfaces are isolated from the complex experimental environment as much as possible through components such as metal mesh, metal sleeves, plastic insulating platforms, and metal shells, reducing background interference signals and facilitating the detection of weak fluorescence signals.

[0033] (3) This invention uses a double gold mesh at the top of the detector instead of the traditional single gold mesh structure to filter interference signals. By applying positive and negative voltages to the two gold meshes respectively, it achieves simultaneous shielding of positive ions and negative electrons, solving the problem that the single gold mesh can only shield a single interfering particle. In addition, the voltage of the second gold mesh is consistent with the voltage of the upper electrode of the photomultiplier tube, so that there is no additional outward electric field between the gold mesh and the photomultiplier tube, avoiding the signal loss caused by the emission of secondary electrons generated after the light shines on the multiplier tube, and further improving the fluorescence detection efficiency. Third, in order to shield the photoelectron signal, the single gold mesh configuration of the traditional detector needs to apply a negative high voltage of hundreds to thousands of volts to the gold mesh, resulting in a high electric field pointing towards the detector between the sample and the detector, which hinders the emission of electrons on the sample and greatly attenuates the intensity of the simultaneously detected total electron yield mode signal (i.e., compensation current). The double gold mesh used in this invention applies a positive voltage of zero to tens of volts at the first gold mesh near the sample, which does not suppress the emission of photoelectrons at the sample, and helps to collect the total electron yield and total fluorescence yield signals simultaneously in the experiment.

[0034] (4) This invention uses a spring and double nuts to fix the wires connecting the photomultiplier tube electrodes, replacing the traditional screw and washer method. There are three advantages: First, the photomultiplier tube fixing end is a ceramic part, and the spring compression method makes the pressure increase during tightening smoother, avoiding the damage to the ceramic part caused by sudden pressure changes during traditional screw fixing; second, by selecting a spring with appropriate elastic coefficient and length and using a screw of a specific length, the spring force can be locked, which helps improve the repeatability of pressure when different personnel replace the photomultiplier tube, reducing human error during installation; third, the double-nut tightening method prevents the wires from loosening under vibration conditions, ensuring the normal operation of the detector under complex in-situ experimental conditions. Attached Figure Description

[0035] Figure 1 This is a schematic diagram of the main components of the all-fluorescent yield detector for in-situ soft X-ray absorption spectroscopy of the present invention;

[0036] Figure 2 This is a schematic diagram of an interference signal shielding mesh assembly.

[0037] Figure 3 Figure (a) is a front view, (b) is a bottom view, and (c) is a sectional view.

[0038] Figure 4 This is a schematic diagram of a fluorescence signal receiver assembly;

[0039] Figure 5 The diagram shows some components of the fluorescence signal receiver assembly, where Figure (a) shows the photomultiplier tube fixing component and Figure (b) shows the photomultiplier tube.

[0040] Figure 6 This is a schematic diagram of the shielding and support components;

[0041] Figure 7 A front view of the semi-cylindrical shell in the shielding and support assembly;

[0042] Figure 8 Schematic diagram of electrical connections and external sealing components;

[0043] Figure 9 Figure 1 shows a schematic diagram of some components in the electrical connection and external sealing assembly. Figure 2 shows a cross-sectional view of the wire connector, Figure 3 shows an isometric view of the insulation support platform, Figure 4 shows a top view of the insulation support platform, Figure 5 shows an isometric view of the housing connector, and Figure 6 shows a top view of the housing connector.

[0044] Figure 10 This is a schematic diagram showing the positional relationship between the detector and the sample.

[0045] Figure 11 This is a schematic diagram of the electrical connections of the detector. Detailed Implementation

[0046] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention. Furthermore, the technical features involved in the various embodiments of this invention described below can be combined with each other as long as they do not conflict with each other.

[0047] The all-fluorescence yield detector for in-situ soft X-ray absorption spectroscopy of the present invention consists of four parts, such as... Figure 1 As shown, the assembly includes an interference signal shielding mesh assembly 1, a fluorescent signal receiver assembly 2, a shielding and support assembly 3, and an electrical connection and external sealing assembly 4. The interference signal shielding mesh assembly 1, the fluorescent signal receiver assembly 2, and the electrical connection and external sealing assembly 4 are sequentially fastened to the shielding and support assembly 3. The key components of each of the four parts will be described below.

[0048] like Figure 2 As shown, the interference signal shielding mesh assembly 1 mainly consists of an aluminum annular electrode 1-1, a gold mesh 1-2, an insulating ring 1-3, a first high-voltage conductor 1-4, an outer insulating sleeve 1-5, an insulating screw 1-6, and an internal hex screw 1-7. The two layers of gold mesh 1-2 are separated by the insulating ring 1-3. The voltage on the gold mesh 1-2 is provided by the first high-voltage conductor 1-4 fixed to the aluminum annular electrode 1-1. The first high-voltage conductor 1-4 is fastened inside the aluminum annular electrode 1-1 by the internal hex screw 1-7. The aluminum annular electrode 1-1, the gold mesh 1-2, and the insulating ring 1-3 form a "sandwich" structure, which is then fastened to the outer insulating sleeve 1-5 by the insulating screw 1-6.

[0049] The aluminum ring electrode 1-1 is a hollow metal ring with a threaded hole. The material is aluminum, the model is 6061, and there are 2 of them. Its functions include: (1) cooperating with the insulating ring 1-3 and the insulating screw 1-6 in the middle to fix the gold mesh 1-2; (2) acting as an electrode to contact the first high voltage wire 1-4 to provide voltage to the gold mesh 1-2.

[0050] The gold mesh 1-2 is a 90% light transmittance mesh made of pure gold, and there are two of them. Its function is as follows: the upper first layer of gold mesh 1-2a operates under a positive voltage to shield positive ions in the experimental device, and the lower second layer of gold mesh 1-2b operates under a negative high voltage to form a near-parallel electric field between the two layers of gold mesh 1-2, which is used to shield photoelectrons generated after the sample is irradiated with X-rays.

[0051] The insulating ring 1-3 is a hollow plastic ring made of polyether ether ketone (PEEK), and there is one ring. Its functions include: (1) fixing the gold mesh 1-2 in conjunction with the aluminum ring electrode 1-1 and the insulating screw 1-6; (2) insulating the two aluminum ring electrodes 1-1.

[0052] The first high-voltage conductor 1-4 is a conductor with an external insulation layer. The insulation layer material is polyimide, and the conductor core material is silver-plated copper wire. There are 2 conductors, and their functions include: (1) The upper end of the first high-voltage conductor 1-4a connected to the first gold mesh is connected to the upper ring electrode 1-1a, and the lower end is connected to the external power supply to provide a positive voltage for the first gold mesh 1-2a; (2) The upper end of the first high-voltage conductor 1-4b connected to the second gold mesh is connected to the lower ring electrode 1-1b, and the lower end is connected to the upper electrode of the photomultiplier tube 2-2 to provide a negative high voltage for the second gold mesh 1-2b.

[0053] The outer insulating sleeves 1-5 are as follows Figure 3 As shown, it is a hollow conical top cylinder made of polyetheretherketone (PEEK), with a quantity of 1. Its functions include: (1) insulating the high-voltage connecting parts such as the gold mesh 1-2 and other parts of the detector; (2) preventing the gold mesh 1-2 from contacting the sample and causing a short circuit hazard when the detector is in use. In addition, the front end of the outer insulating sleeve 1-5 adopts a 30° conical design, which can make the light incident from the side as unobstructed as possible and increase the working range of the detector.

[0054] The insulating screws 1-6 are made of polyetheretherketone (PEEK) and there are 4 of them. Their function is to cooperate with the aluminum ring electrode 1-1 and the insulating ring 1-3 to fix the gold mesh 1-2 onto the outer insulating sleeve 1-5.

[0055] The internal hex screws 1-7 are made of stainless steel, model 304, and there are 2 of them. Their function is to cooperate with the aluminum ring electrode 1-1 to fix the first high-voltage wire 1-4.

[0056] like Figure 4As shown, the fluorescence signal receiver assembly 2 is the core component of this detector. It mainly consists of a photomultiplier tube holder 2-1, a photomultiplier tube 2-2, a rubber pad 2-3, first fastening screws 2-4, gold-plated screws 2-5, washers 2-6, a spring 2-7, a second high-voltage wire 2-8, a signal wire 2-9, and a fastening nut 2-10. Three first fastening screws 2-4 are placed on the rubber pad 2-3 to fix the photomultiplier tube 2-2 to the holder 2-1. Two gold-plated screws 2-5 are connected to the electrodes of the photomultiplier tube 2-2. The spring 2-7 is separated from the lower surface of the photomultiplier tube 2-2 by the washers 2-6. The second high-voltage wire 2-8 is then connected in series with the gold-plated screws 2-5 via a gold-plated copper terminal, and finally secured with the fastening nut 2-10. The output signal of the photomultiplier tube 2-2 is led out through the signal wire 2-9 at the end, which is also secured with the fastening nut 2-10.

[0057] like Figure 5 As shown, the multiplier tube fixing component 2-1 is a cylindrical truncated cone with a central stepped surface (e.g., Figure 5 Figure (a) shows that the material is polyether ether ketone (PEEK), the quantity is 1, and the functions include: (1) fixing the photomultiplier tube 2-2 through the threaded hole on the middle step surface and the first fastening screw 2-4; (2) supporting the entire fluorescent signal receiver assembly 2 by connecting to the shielding and support assembly 3 through the threaded hole on the cylindrical surface.

[0058] The photomultiplier tube 2-2 is a photomultiplier tube with a tapered receiving port (e.g., ...). Figure 5 Figure (b) shows a single photomultiplier tube (2-2). Its outer wall is primarily made of ceramic, with gold electrodes plated at the conical opening and lower part for applying high voltage. The inner wall is made of lead glass with an S-shaped channel for photoelectric signal gain. A small screw is located at the bottom of the photomultiplier tube 2-2 for collecting the gain signal and connecting to the signal line. Figure 5 Figure (b) shows the functions of different holes on photomultiplier tube 2-2: a1 represents the upper electrode, a2 represents the lower electrode, a3 represents the signal terminal, and a4 represents the photomultiplier tube fixing hole.

[0059] The rubber pad 2-3 is an L-shaped perforated thin rubber pad made of fluororubber, and there is one pad in total. Three through holes are provided at the top corner to cooperate with the first fastening screw 2-4. Its functions include: (1) increasing friction to prevent the screw from loosening; (2) using the elasticity of the rubber to prevent the ceramic body from cracking due to sudden increase in force during fastening; and (3) reducing the wear on the ceramic surface of the photomultiplier tube 2-2 body when installing the first fastening screw 2-4.

[0060] The first fastening screw 2-4 is made of stainless steel, model 304, with gold plating, and there are 3 of them. Its function is to fix the rubber pad 2-3 and the photomultiplier tube 2-2 to the multiplier tube fixing part 2-1 in sequence, with the bottom surface of the multiplier tube in contact with the step surface.

[0061] The gold-plated screws 2-5 are made of stainless steel, model 304, and are gold-plated. There are 2 of them. Gold plating can reduce the surface resistance of the screws and improve their conductivity. Their function is to connect with the second high-voltage wire 2-8 and the photomultiplier tube electrode to provide voltage for the photomultiplier tube 2-2.

[0062] The gaskets 2-6 are made of stainless steel, model 304, with gold plating, and there are 6 of them. Their function is to increase the contact area when installing the gold-plated screws 2-5 and springs 2-7, and to prevent the edges of the gold-plated screws 2-5 and springs 2-7 from directly contacting the photomultiplier tube 2-2, which would generate excessive pressure and damage the main ceramic component.

[0063] The springs 2-7 are made of beryllium copper, plated with gold, and number two. They are separated at both ends by washers 2-6 and installed on gold-plated screws 2-5. Their functions include: (1) providing appropriate pressure to the contact surface between the gold-plated screws 2-5 and the multiplier tube electrode; (2) by selecting appropriate spring length and hardness, and matching the length of the gold-plated screw, the installation pressure can be kept close each time, reducing human installation errors.

[0064] The second high-voltage conductor 2-8 is a conductor with an external insulation layer. The insulation layer material is polyimide, and the conductor core material is silver-plated copper wire. There are 2 conductors, and their functions include: (1) The second high-voltage conductor 2-8a connected to the negative electrode and the first high-voltage conductor 1-4b connected to the second layer of gold mesh are connected in series through gold-plated screw 2-5. The series connection is transitioned by connecting gold-plated copper terminals, and the lower ring electrode, the upper electrode of the photomultiplier tube 2-2 and the external power supply are connected to provide the same negative high voltage to the front end of the photomultiplier tube 2-2 and the second layer of gold mesh 1-2b; (2) The second high-voltage conductor 2-8b connected to the positive electrode connects the lower electrode of the photomultiplier tube 2-2 and the external power supply to provide voltage to the rear end of the photomultiplier tube 2-2.

[0065] The signal line 2-9 is a double-shielded wire with an external insulation layer. The insulation layer material is polyimide, the shielding mesh is stainless steel braided mesh, and the wire core material is silver-plated copper wire. It is connected to a gold-plated copper terminal for fixation. There is one terminal, and its function is to connect the signal end of the photomultiplier tube 2-2 to the external signal receiver and draw out the photocurrent generated by the photomultiplier tube 2-2.

[0066] The fastening nuts 2-10 are made of stainless steel, model 304, with gold plating, and there are 6 of them. Their functions include: (1) dividing into three groups, fastening the two second high-voltage wires 2-8 and signal wires 2-9 by double nuts, and connecting them to the multiplier tube electrodes and signal terminals with the screw; (2) adjusting the position of the fastening nuts, and adjusting the contact tightness of the multiplier tube electrodes with the spring 2-7.

[0067] like Figure 6 As shown, the shielding and support assembly 3 includes two parts: a semi-cylindrical housing 3-1 and a countersunk screw 3-2. The countersunk screw 3-2 acts as a fastener to connect the semi-cylindrical housing 3-1, the outer insulating sleeve 1-5, the multiplier tube fixing piece 2-1, and the housing connector 4-5, thereby supporting and positioning the detector as a whole.

[0068] The semi-cylindrical outer shell 3-1 is made of stainless steel, model 316L, and has a semi-cylindrical shape, with two in number. Three sets of through holes are provided on the outer shell, with each set of holes spaced 90° apart. Figure 7 The different hole positions on the semi-cylindrical shell are marked, b1 is the fixed position of the interference signal shielding mesh component 1, b2 is the fixed position of the fluorescence signal receiver component 2, and b3 is the fixed position of the electrical connection and external sealing component 4. Its functions include: (1) fixing the interference signal shielding mesh component 1, the fluorescence signal receiver component 2 and the electrical connection and external sealing component 4 from top to bottom with countersunk screws 3-2, ensuring their relative positional relationship and supporting each component; (2) splicing the shell to form a metal cylinder, which, together with the first layer of gold mesh and the lower fixed base, forms a Faraday cage to shield external electromagnetic interference and prevent electrons and positive ions in the vacuum cavity from reaching the multiplier signal end, ensuring the purity of the fluorescence signal.

[0069] The countersunk screws 3-2 are made of stainless steel, type 304, and there are 12 of them. Their function is to connect the semi-cylindrical outer shell 3-1 with the interference signal shielding mesh assembly 1, the fluorescent signal receiver assembly 2, the electrical connection and outer sealing assembly 4.

[0070] like Figure 8As shown, the electrical connection and external sealing assembly 4 is assembled from a high-voltage electrical feeder 4-1, a wire connector 4-2, a metal sleeve 4-3, an insulating support platform 4-4, a housing connector 4-5, second fastening screws 4-6, and a support platform positioning screw 4-7. The housing connector 4-5 is mounted on the insulating support platform 4-4 by four second fastening screws 4-6, and then mounted on the high-voltage electrical feeder 4-1 by the support platform positioning screw 4-7. The wire connector 4-2 mates with the four pins on the high-voltage electrical feeder 4-1. The metal sleeve 4-3 has a clearance fit with the pins and flange surface on the high-voltage electrical feeder. The high-voltage wire and signal wire pass through the through holes on the insulating support platform 4-4 and the housing connector 4-5 and are inserted into the wire connector 4-2. The internal hex screws on the side of the wire connector 4-2 are tightened to fix the four wires.

[0071] like Figure 9 The diagram shows some parts of the electrical connection and external sealing assembly 4. Among them, Figure 9 In Figure (a), a1 is the wire inlet and a2 is the pin inlet of the high-voltage electrical feeder 4-1; Figure 9 Figure (b) is an isometric view of the insulating support platform;

[0072] Figure 9 Figure (c) is a top view of the insulating support platform 4-4, which, from the center outwards, consists of: a central through hole c1, four threaded holes c2, and four first through holes c3. Figure 9 Figure (d) is an isometric view of the housing connector 4-5; Figure 9 Figure (e) is a top view of the housing connector 4-5, which consists of a central through hole c1, four countersunk holes e2, and four second through holes e3, arranged from the center outwards.

[0073] The main body of the high-voltage electrical feeder 4-1 is made of 304 stainless steel. It has a knife-edge flange on the upper part, model DN40CF, and four high-voltage electrode pins on the lower part, model SHV. The center material of the pins is chrome-plated 304 stainless steel, and the insulating material between the pins and the main body is alumina. The center of the flange face has a threaded hole. Its functions are: (1) The electrode pins cooperate with the wires to connect the internal photomultiplier tube and gold mesh to the external power supply and signal receiver to realize the transmission of electrical signals and the application of voltage; (2) The threaded hole in the center of the flange face cooperates with the positioning screw 4-7 of the support platform to fix the support part as a whole to the inner flange face.

[0074] The wire connector 4-2 is made of gold-plated beryllium copper, and there are four of them. Figure 9 As shown in Figure (a), it is a hollow cylinder with a groove at the bottom and a threaded hole on the upper side. Its functions are: (1) to connect the upper part to the wire and fix it with an internal hex screw; (2) to connect the lower part to the pin of the high voltage electrical feeder 4-1.

[0075] The metal sleeve 4-3 is made of oxygen-free copper, gold-plated, and there are four of them. It is a hollow cylinder with fine grooves. Its function is as follows: The pin of the high-voltage electrical feed 4-1 has a circular groove around it. Inserting the metal sleeve 4-3 into the groove forms a grounding shield to prevent scattered electrons and positive ions in the vacuum from contacting the wire connector 4-2 and causing interference.

[0076] The insulating support platform 4-4 is made of polyetheretherketone (PEEK) and is 1 in number. Figure 9 As shown in Figure (b), it is a cylinder with a slotted bottom and threaded holes and through holes at the top. Its functions are: (1) The central through hole, in conjunction with the positioning screw, connects the insulating support platform 4-4 to the flange face of the high-voltage electrical feeder 4-1 and positions it to the center; (2) The threaded hole, in conjunction with the second fastening screw 4-6, connects the fixed base to the insulating support platform 4-4; (3) The four through holes are respectively used to pass through the first high-voltage conductor 1-4a connected to the first layer of gold mesh, the second high-voltage conductor 2-8 and a signal line 2-9, reducing signal interference at the joint.

[0077] The outer casing connectors 4-5 are made of polyetheretherketone (PEEK), and there is one such connector. Figure 9 As shown in Figure (c), it is a cylinder with holes. Its functions are: (1) The through hole is used to pass through the first high voltage conductor 1-4a, the second high voltage conductor 2-8 and the signal line 2-9 connected to the first layer of gold mesh; (2) The stepped through hole is used to cooperate with the second fastening screw 4-6 to fix the outer shell connector 4-5 to the insulating support platform 4-4; (3) The center through hole is used to fix the outer shell connector 4-5 and the insulating support platform 4-4 to the high voltage electrical feedthrough 4-1 through the support platform positioning screw 4-7; (4) The side threaded hole is used to connect with the semi-cylindrical outer shell 3-1 and cooperate with the shielding and support assembly 3.

[0078] The second fastening screw 4-6 is made of stainless steel, type 304, and there are 4 of them. Its function is to connect the outer shell connector 4-5 and the insulating support platform 4-4.

[0079] The positioning screw 4-7 of the support platform is made of stainless steel, model 304, with a silver-plated surface, and there is one screw. Its function is to fix the outer shell connector 4-5 and the insulating support platform 4-4 to the center of the flange face of the high-voltage electrical feeder 4-1.

[0080] Example

[0081] A. Design requirements and scope of application of this invention:

[0082] (1) The working temperature range is from room temperature to 70℃, and the maximum baking temperature is 200℃;

[0083] (2) The detector mounting flange size is DN40CF, the inner diameter of the vacuum pipe is not less than 38mm, and the vacuum level of the cavity during operation is better than 1×10⁻⁶. -7 mbar;

[0084] (3) The number of flange interfaces of the high voltage electrical feeder 4-1 shall not be less than 4, and the withstand voltage shall not be less than 3kV;

[0085] (4) The length from the top of the detector to the flange surface can be customized according to requirements within the range of 100-400mm;

[0086] (5) Figure 10 As shown, based on the characteristics of in-situ experiments, the fluorescence emission range is approximately a cone angle of 70°. Therefore, the detector design needs to be as close to the sample as possible to increase the receiving angle, while not blocking the X-rays incident on the sample. This invention can simultaneously meet the two requirements: a) a distance of 40 mm from the sample and b) a minimum angle of 30° with the incident X-rays, thus satisfying the detection requirements of in-situ experiments.

[0087] B. Specific connection and configuration methods of the present invention:

[0088] (1) Detector electrical connections are as follows Figure 11 As shown, A, B, C, and D correspond to the four interfaces of the flange of the high-voltage electrical feedthrough 4-1: (a) A is connected to the first layer of gold mesh and a positive voltage (0 to +100V) is applied, mainly to shield positive ions in the vacuum chamber; (b) B is connected to the second layer of gold mesh and the negative terminal of the front end of the photomultiplier tube 2-2 and a negative high voltage (-400 to -2500V) is applied. The negative voltage of the second layer of gold mesh is used to shield photoelectrons emitted from the sample, and the negative terminal of the photomultiplier tube 2-2 is used to form a voltage drop between the positive and negative terminals to amplify the secondary electrons excited by the incident light irradiating the photomultiplier tube 2-2; (c) C is connected to the 4MΩ resistor R and the negative terminal of the photomultiplier tube 2-2, with its outer end grounded. Through resistor voltage division, the potential at the C terminal is made to be about 10 to 100V lower than that at the ground terminal, ensuring that the amplified electrons are concentrated towards D (signal terminal) under the influence of the electric field, which helps to improve signal collection efficiency; (d) D is connected to the signal terminal for signal reception and transmission.

[0089] (2) The detector facing the sample end uses a pure gold mesh with 90% transmittance to filter interference signals, and the chemical stability of gold is used to cope with the complex acid, alkali and organic environment of the in-situ experiment.

[0090] (3) Using polyetheretherketone (PEEK) as the main insulating material is suitable for the precision machining of non-standard parts required by this invention and for the long-term operation of the detector under high voltage.

[0091] (3) Aluminum, silver-plated copper wire, gold electrode plating, etc. are used as electrical contact and electrical signal transmission materials to ensure high conductivity;

[0092] (4) SHV type connectors are used for high-voltage electrical connections to meet the voltage requirement of up to 3kV;

[0093] (5) 316L stainless steel and polyether ether ketone (PEEK) are used as the outer surface structural materials of the detector, which are stable to acid, alkali and organic environments and adaptable to a variety of in-situ experimental environments;

[0094] (6) Flexible Viton rubber and screws are used to fix the photomultiplier tube, which ensures good electrical contact and avoids damage to ceramic parts caused by sudden changes in hard contact pressure when fixing the multiplier tube.

[0095] (7) A Faraday cage is formed by using a stainless steel shell, a metal shell, and aluminum connectors for the bottom shell to physically and electromagnetically shield external interference signals, ensuring the reliability of the signal during fluorescence reception and gain, and reducing background noise.

[0096] (8) The modular design is adopted, and the interference signal filter, fluorescent signal receiver and sealing components are designed as modules that can be independently disassembled and combined. The equipment can be maintained and upgraded by replacing the modules.

[0097] (9) The traditional L-shaped bracket or hollow tube is replaced by splicing two semi-cylindrical stainless steel shells for support and component fixation. The internal parts can be maintained by disassembling one of the semi-cylindrical shells.

[0098] (10) The wires and electrodes are connected by using ring-shaped metal terminals with screws and nuts, pin-type flexible connectors and SHV standard connectors, which can achieve quick assembly and disassembly.

[0099] C. Assembly of the parts and components of the present invention:

[0100] After the detector of the present invention is assembled, it is connected to the vacuum chamber through the knife-edge flange of the high-voltage electrical feed 4-1.

[0101] D. The specific process of in-situ detection of the full fluorescence yield absorption spectrum of a sample:

[0102] (1) Place the sample in the in-situ reaction environment to achieve the required operating state;

[0103] (2) Soft X-rays are irradiated onto the surface of the sample in a normal incidence manner;

[0104] (3) The detector is moved to a distance of 40 mm from the sample by the displacement mechanism;

[0105] (4) Turn on the high voltage power supply and signal acquisition system. Depending on the research system, first apply the required positive voltage to the first layer of gold mesh, and then gradually increase the negative high voltage at the front electrode of the second layer of gold mesh / photomultiplier tube. Observe the change in signal strength after gain.

[0106] (5) After the signal intensity reaches the required gain range, adjust the incident soft X-ray energy within the required detection energy range and record the signal intensity change to obtain the full fluorescence yield absorption spectrum.

[0107] Preferably, the present invention uses two semi-cylindrical shells, which can be replaced with semi-prismatic surfaces or other shapes, the purpose of which is to form a Faraday cage and provide support;

[0108] Preferably, the semi-cylindrical outer shell material in this invention is 316L stainless steel, but it can also be replaced with other machinable conductor materials such as aluminum or copper, depending on the usage environment.

[0109] Preferably, the material of the interference signal shielding mesh in this invention is pure gold, but it can also be replaced with metals such as copper, nickel, and stainless steel, depending on the usage environment.

[0110] Preferably, the present invention uses polyetheretherketone, polyimide, and alumina ceramic as insulating materials, but can also be replaced with other insulating materials such as polytetrafluoroethylene, boron nitride, and aluminum nitride ceramic.

[0111] Preferably, the present invention uses polyetheretherketone and stainless steel for precision machining of non-standard parts. Depending on the usage environment, it can also be replaced by materials that can be machined and have the required mechanical strength, such as titanium alloy, aluminum, copper, polyimide, mica, and ceramics.

[0112] Preferably, the photomultiplier tube used in this invention has a collection port diameter of 20 mm, but it can be replaced with other sizes between 10 and 25 mm as needed;

[0113] Preferably, the voltage divider resistor connected to the photomultiplier tube of the present invention has a resistance of 4MΩ, and its resistance can vary depending on the model of the photomultiplier tube.

[0114] Preferably, the method used to connect the photomultiplier tube electrode and the signal terminal in this invention is for DC signal acquisition. Depending on the type and frequency of the acquired signal, it can be replaced by other connection methods that use diodes, capacitors, etc.

[0115] Preferably, the gold mesh used in this invention has a thickness of 20 μm, but it can be replaced with other thicknesses as needed;

[0116] Preferably, the voltage range of the first gold mesh in this invention is 0 to +100V, which is suitable for most environments in in-situ experiments. Depending on the energy of the positive ions to be shielded, it can also be replaced with a higher voltage.

[0117] Preferably, the distance between the two gold mesh layers in this invention is 3mm, but it can be adjusted to other distances according to requirements such as voltage range;

[0118] Preferably, in this invention, the gold-plated screw and nut connecting the photomultiplier tube electrode is M1.6, 12mm in length, and made of stainless steel. The spring has a free length of 3.5mm, a diameter of 0.2mm, and is also made of stainless steel. The dimensions of the screw and spring can be adjusted according to the photomultiplier tube hole position and fixing pressure requirements, and the spring material can also be replaced with other elastic materials such as high-carbon spring steel, stainless steel, titanium, and special alloys.

[0119] Preferably, the present invention connects the second layer of gold mesh and the front electrode of the photomultiplier tube, but it can also be replaced by connecting the two independently to different high-voltage power supplies. Accordingly, the number of high-voltage electrical feedthrough terminals can be increased;

[0120] Preferably, the signal line and high-voltage conductor material used in this invention is silver-plated copper, which can be replaced by copper wire, silver wire, aluminum wire or other conductive materials;

[0121] Preferably, in order to meet the requirements of modular design, insulation and convenient installation, the outer shell connector and the insulating support platform are divided into two parts. According to actual needs, the two can be replaced into one part, and the material can be metal or machinable plastic.

[0122] Preferably, the lengths of the support components such as the semi-cylindrical shell, the insulating support platform, and the top outer insulating sleeve in this invention can be adjusted according to different experimental chamber dimensions and can be replaced with other lengths;

[0123] Preferably, the cone angle of the top outer insulating sleeve in this invention is 30°, but it can be replaced with other values ​​between 0° and 90° depending on the requirements of the soft X-ray incident angle and the fluorescence divergence angle.

[0124] Preferably, the buffer material used to fix the photomultiplier tube in this invention is fluororubber, but it can also be replaced with other flexible buffer materials such as silicone rubber and polytetrafluoroethylene.

[0125] Preferably, the electrical interface model of the high-voltage electrical feedthrough used in this invention is SHV, and the quantity is 4. It can also be replaced by a non-standard interface with 3 SHV and 1 BNC interface.

[0126] Preferably, the present invention uses a CF knife-edge flange as the external sealing element. Depending on the vacuum requirements, other sealing methods such as KF flanges can also be used.

[0127] Those skilled in the art will readily understand that the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A total fluorescence yield detector for in-situ X-ray absorption spectroscopy, characterized in that, The interference signal shielding net assembly, the fluorescent signal receiver assembly, the shielding and supporting assembly, and the electrical connection and outer sealing assembly are provided. The interference signal shielding net assembly comprises an aluminum ring electrode, a gold net, an insulating ring, a first high-voltage wire, an outer insulating sleeve, an insulating screw, and an internal hexagonal screw. The fluorescent signal receiver assembly comprises a multiplier tube fixing part, a photomultiplier tube, a rubber pad, a first fastening screw, a gold-plated screw, a gasket, a spring, a second high-voltage wire, a signal wire, and a fastening nut. The shielding and supporting assembly comprises a semi-cylindrical shell and a countersunk screw. The countersunk screw is used as a fastener to connect the semi-cylindrical shell and the outer insulating sleeve, the multiplier tube fixing part, and the shell connecting part to support and position the whole detector. The electrical connection and outer sealing assembly is assembled by a high-voltage electrical feedthrough, a wire joint, a metal sleeve, an insulating support platform, a shell connecting part, a second fastening screw, and a support platform positioning screw.

2. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The aluminum ring electrode is a hollow ring with threaded holes.

3. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The gold net has a 90% light transmittance.

4. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The insulating ring is a hollow ring. The outer insulating sleeve is a hollow conical top cylindrical. The internal hexagonal screw is made of stainless steel. The gold net is made of pure gold, and the thickness of the gold net is 20μm. The distance between the two layers of gold nets is 3mm. The end facing the sample uses a 90% transmittance gold net to filter interference signals. The top angle of the outer insulating sleeve is 0°-90°.

5. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The multiplier tube fixing part is a cylindrical platform with a middle step surface; the photomultiplier tube is provided with a tapered receiving port; the rubber pad is an L-shaped thin rubber pad with a hole; the two ends of the spring are separated by a gasket and installed on a gold-plated screw; the second high-voltage wire is a wire with an external insulating layer; and the signal wire is a double-shielded wire with an external insulating layer.

6. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The photomultiplier tube is fixed to the multiplier tube fixing part by using a flexible rubber pad and a first fastening screw, thereby ensuring good electrical contact and avoiding damage to the ceramic part caused by sudden hard contact pressure when the photomultiplier tube is fixed.

7. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The gold-plated screw and the fastening nut are M1.6, 12 mm in length, and made of stainless steel; the spring has a free length of 3.5 mm, a diameter of 0.2 mm, and is made of stainless steel, high-carbon spring steel, stainless steel, titanium or special alloy; the size of the gold-plated screw and the spring can be adjusted according to the hole position of the photomultiplier tube and the fixing pressure requirement; the ring-shaped metal terminal is used in combination with the fastening nut to connect the second high-voltage wire and the gold-plated screw, and quick disassembly and assembly can be realized.

8. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The upper part of the high-voltage electrical feedthrough is provided with a knife flange, and the lower part is provided with four high-voltage electrode pins; the wire joint is a hollow cylinder, the lower part of the cylinder is provided with a fine groove, and the upper part is provided with a threaded hole; the metal sleeve is a hollow cylinder with a fine groove; the insulating support platform is a cylinder with a slotted bottom, and the upper part is provided with a threaded hole and a through hole; and the shell connecting piece is a cylindrical piece with a hole.

9. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, A Faraday cage is formed by using a semi-cylindrical shell made of stainless steel, a gold-plated metal sleeve and an aluminum shell connecting piece to physically and electromagnetically shield external interference signals, ensure the reliability of the signals in the fluorescence receiving and gain process, and reduce background noise; the material of the semi-cylindrical shell is 316L stainless steel, aluminum or copper.

10. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The electrical connection of the detector is as follows: The flange of the high-voltage electrical feedthrough includes interfaces A, B, C and D; the interface A is connected with the first layer of gold mesh and is applied with a positive voltage in the range of 0-+100V, which is used to shield positive ions in the vacuum cavity; the interface B is connected with the second layer of gold mesh and the front negative electrode of the photomultiplier tube and is applied with a negative high voltage in the range of -400--2500V, the negative voltage of the second layer of gold mesh is used to shield photoelectrons emitted from the sample, and the negative electrode of the photomultiplier tube is used to form a voltage drop between the positive and negative electrodes to gain the secondary electrons excited by the incident light on the photomultiplier tube; the interface C is connected with the 4MΩ resistor R and the negative electrode of the photomultiplier tube, and the outer end is grounded, the potential at the interface C is 10-100V lower than the ground end through voltage division by the resistor, which ensures that the electrons after gain are gathered to the interface D connected with the signal end by the action of the electric field, which helps to improve the signal collection efficiency; the interface D is connected with the signal end and is used for signal receiving and transmission.

11. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The working temperature range is from room temperature to 70℃, the maximum baking temperature is 200℃, the flange size of the detector is DN40CF, the inner diameter of the vacuum pipeline is not less than 38mm, the cavity vacuum degree during operation is better than 1×10 -7 mbar, the number of flange interfaces of the high-voltage electrical feedthrough is not less than 4, the voltage resistance is not less than 3kV, the length from the top of the detector to the flange surface is within the range of 100-400mm, and can be customized according to requirements, the fluorescence exit range is a cone angle of 70°, and at the same time, the distance from the sample is 40mm and the minimum angle between the incident X-ray and the detector is 30°, thereby meeting the in-situ experiment detection requirements.

12. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, Polyether ether ketone, polyimide and aluminum oxide ceramic are used as insulating materials, or polytetrafluoroethylene, boron nitride and aluminum nitride ceramic are used as insulating materials.

13. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, Polyether ether ketone and stainless steel are used for precision machining of non-standard parts, or titanium alloy, aluminum, copper, polyimide, mica and ceramic are used as materials that can be machined and have the required mechanical strength according to the use environment.

14. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The gold mesh is replaced by copper, nickel or stainless steel, and the thickness of the single layer mesh and the distance between the two layers of metal mesh can be adjusted according to requirements.

15. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The top taper angle of the outer insulation sleeve is 30°.

16. A total fluorescence yield detector for in situ X-ray absorption spectroscopy according to claim 1, characterized in that, The semi-cylindrical shell is replaced by a semi-prismatic shell to form a Faraday cage and provide support.

Citation Information

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