CN111024732B - Dynamic in-situ gas phase reaction tank for soft X-ray spectroscopy experiment - Google Patents
Dynamic in-situ gas phase reaction tank for soft X-ray spectroscopy experiment Download PDFInfo
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- CN111024732B CN111024732B CN201911421849.5A CN201911421849A CN111024732B CN 111024732 B CN111024732 B CN 111024732B CN 201911421849 A CN201911421849 A CN 201911421849A CN 111024732 B CN111024732 B CN 111024732B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/03—Investigating materials by wave or particle radiation by transmission
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
Abstract
The invention provides a dynamic in-situ gas phase reaction tank for a soft X-ray spectroscopy experiment, which comprises a reaction tank main body, a reaction tank supporting piece and an external connecting piece, wherein the reaction tank main body is provided with a plurality of reaction tanks; the reaction tank main body is provided with a sample cavity for placing a sample and a first light through hole communicated with the sample cavity, and a metal partition plate is arranged in the sample cavity; the reaction tank support piece comprises a support pipe, and the support pipe is connected with the reaction tank main body; the external connecting piece comprises a connector, a differential pumping pipeline, an electronic yield signal line and a bias line, wherein one end of the bias line sequentially penetrates through the differential pumping pipeline, the connector, a supporting pipe and the reaction tank main body to be connected with the metal partition plate. The invention applies bias voltage to the metal clapboard, so that an electric field is generated between the sample and the metal clapboard, and ionized gas particles are pulled away from the surface of the sample, thereby reducing background noise and making the collection of an electronic yield signal possible; the reasonable Reynolds coefficient is achieved by reducing the distance between the window and the sample and adjusting the gas flow rate, so that the gas renewal speed on the surface of the material is high.
Description
Technical Field
The invention relates to the technical field of in-situ experiments, in particular to a dynamic in-situ gas phase reaction tank for soft X-ray spectroscopy experiments.
Background
In the field of scientific research, in-situ experiment refers to an experimental method for simulating a real environment and tracking and observing the changes of the structure, the property and the like of an experimental object while a scientific phenomenon occurs. The core component for carrying out in situ experiments is called an in situ reaction cell, and the main function of the in situ reaction cell is to load a sample and simulate reaction conditions.
Soft X-ray spectroscopy is a powerful tool for studying the electronic structure change of materials, the energy range of soft X-rays is defined as 100-2000eV, the energy required by detecting the K-edge absorption edge of a light element and the L-edge absorption edge of a transition metal element is included, and the penetration depth of the X-rays in the energy range in substances is shallow, so that the design difficulty of a reaction tank is higher compared with other energy ranges. The existing in-situ reaction tank has three main problems: firstly, the design of the normal in-situ reaction pool does not consider the collection of an electron yield signal, but generally collects an optical signal, so that the requirement on the structural design of the reaction pool is greatly reduced; compared with optical signals, electronic signals are more sensitive in surface, so that the collection of the electronic signals is crucial to the research of systems such as catalysis and sensors which mainly react at gas and material interfaces, and the traditional reaction tank cannot effectively collect the interface electronic signals; secondly, the influence of factors such as conductance and the like on a system to be researched is not considered in the design of a general reaction tank, but due to the importance of interface reaction, the gas needs to be kept flowing fast on an interface, so that the product gas is quickly far away from the interface and the product gas is quickly close to a material interface, and therefore the traditional gas channel design cannot meet the observation requirements of the system and needs a more reasonable reaction tank mechanical structure design; thirdly, materials such as polyimide films, aluminum oxide and silicon oxide are generally adopted as observation windows in the existing in-situ reaction tank, the reaction tank can be suitable for in-situ experiments which take infrared rays, visible light and hard X rays as light sources for observation, but because the penetration depth of soft X rays in the materials is small, the material change information in the reaction tank cannot be effectively obtained when the materials are adopted.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a dynamic in-situ gas phase reaction tank which can be used for soft X-ray spectroscopy experiments.
The invention provides a dynamic in-situ gas phase reaction tank for a soft X-ray spectroscopy experiment, which comprises a reaction tank main body, a reaction tank supporting piece and an external connecting piece, wherein the reaction tank main body is provided with a plurality of reaction tanks;
the reaction tank main body is provided with a sample cavity for placing a sample and a first light through hole communicated with the sample cavity, a metal partition plate is arranged in the sample cavity, a second light through hole communicated with the first light through hole is arranged on the metal partition plate, and a light through window matched with the second light through hole is arranged on the inner side of the metal partition plate;
the reaction tank support piece comprises a support pipe, and the support pipe is connected with the reaction tank main body;
the external connecting piece comprises a connector, a differential pumping pipeline, an electronic yield signal line and a bias line, the connector is connected with one end of the supporting tube, which is far away from the main body of the reaction tank, the differential pumping pipeline is connected with the connector, the differential pumping pipeline is provided with a vacuum interface for connecting a vacuum pump, and one end of the electronic yield signal line sequentially penetrates through the connector and the supporting tube to be connected with the reaction tank; one end of the bias line sequentially penetrates through the differential pumping pipeline, the connector, the supporting pipe and the reaction tank main body to be connected with the metal partition plate.
Preferably, the reaction tank main body comprises a reaction tank cover, an insulating sleeve, a metal partition plate and a reaction tank base, the reaction tank cover is provided with a mounting hole and a first light through hole communicated with the mounting hole, the insulating sleeve and the metal partition plate are both arranged in the mounting hole, the metal partition plate is positioned on one side, close to the light through hole, of the insulating sleeve, the insulating sleeve is provided with a sample cavity, and a sample holder for placing a sample is arranged in the sample cavity; the reaction cell base is connected with the reaction cell cover for sealing the sample cavity.
Preferably, the reaction tank cover and the insulating sleeve are made of polyether-ether-ketone materials.
Preferably, one side of the reaction tank base, which is close to the insulating sleeve, is provided with a first pillar which extends into the sample cavity and is used for bearing the sample support; preferably, a first sealing ring is arranged on the connecting surface of the reaction tank base and the reaction tank cover.
Preferably, a second pillar is arranged on one side, close to the insulating sleeve, of the metal partition plate, an annular insulating gasket with a notch is arranged between the light transmission window and the metal partition plate, and a second sealing ring is arranged on the connecting surface of the insulating gasket and the metal partition plate; preferably, a third sealing ring is arranged on the connecting surface of the metal partition plate and the reaction tank cover.
Preferably, the diameters of the first optical through hole and the second optical through hole are gradually reduced from outside to inside, and the aperture angles of the first optical through hole and the second optical through hole are both 120 °.
Preferably, the support tube comprises an adjusting connecting tube and an insulating connecting tube, the length of the adjusting connecting tube is adjustable, two ends of the adjusting connecting tube are respectively connected with a first connecting cover and a second connecting cover, the first connecting cover is provided with a first through hole through which the bias line passes, and the second connecting cover is provided with a second through hole through which the bias line passes; one end of the insulating connecting pipe is connected with the reaction tank base through a screw, and the other end of the insulating connecting pipe is connected with the first connecting cover through a screw; preferably, the insulating connecting pipe is made of polyether-ether-ketone material.
Preferably, the external connecting piece also comprises two gas pipelines, the connectors comprise a main connector, a signal line connector, a bias line connector and two gas pipeline connectors, and the differential pumping pipeline, the signal line connector and the two gas pipeline connectors are all connected with the main connector; one end of an electronic yield signal wire sequentially passes through the signal wire connector, the main connector, the second connecting cover, the adjusting connecting pipe, the first connecting cover and the insulating connecting pipe to be connected and conducted with the reaction tank base, and one ends of the two gas pipelines sequentially pass through the gas pipeline connector, the main connector, the second connecting cover, the adjusting connecting pipe and the first connecting cover to be in threaded connection with the reaction tank base and communicated with the sample cavity; the bias line joint is connected with one end, far away from the main connector, of the differential pumping pipeline, and one end of the bias line sequentially penetrates through the bias line joint, the differential pumping pipeline, the main connector, the second connecting cover, the adjusting connecting pipe, the first connecting cover, the insulating connecting pipe, the reaction tank substrate and the metal partition plate to be connected.
Preferably, the main connector is provided with 1 CF35 flange port and 5 CF16 flange ports, and the main connector is connected with the second connecting cover through the CF35 flange ports;
wherein 3 CF16 flange mouths are uniformly distributed on the back along the circumference of the CF35 flange mouth, the included angle between the 3 CF16 flange mouths and the knife edge flange face of the CF35 flange mouth is 30 degrees, and the signal connector and the two gas pipeline connectors are both CF16 flanges and are respectively connected with the 3 CF16 flange mouths;
the other CF16 flange port and the CF35 flange port are directly communicated, the included angle between the CF16 flange port and the CF35 flange port edge flange face is 180 degrees, and a differential pumping pipeline is connected with the CF16 flange port;
preferably, the main connector is also provided with a spare CF16 flange opening in a sealed state;
preferably, a fourth sealing ring is arranged on the connecting surface of the CF35 flange opening and the second connecting cover.
Preferably, the differential pumping pipeline is a CF16 tee pipeline, the bias line joint is a CF16 flange, a first passage of the differential pumping pipeline is connected with a CF16 flange port, a second passage of the differential pumping pipeline is connected with the bias line joint, and a third passage of the differential pumping pipeline is a vacuum interface for connecting a vacuum pump.
The dynamic in-situ gas phase reaction tank for the soft X-ray spectroscopy experiment provided by the invention adopts the metal partition plate to apply bias voltage, so that an electric field is generated between a sample and the metal partition plate, and ionized gas particles are pulled away from the surface of the sample, thereby reducing background noise and enabling the collection of an electron yield signal to be possible; the invention improves the light intensity reaching the sample surface by reducing the distance between the window and the sample, improves the signal intensity, and achieves reasonable Reynolds coefficient by introducing gas through the gas pipeline and adjusting the gas flow velocity, thereby ensuring the gas renewal speed on the material surface, and meanwhile, as the sample support center is provided with the communicating groove for communicating the central circular groove and the gas channel, the gas can smoothly flow to avoid forming turbulent flow, so the gas renewal efficiency is high, and the invention is beneficial to observing the change of the material and gas interface; the invention adopts silicon nitride, carbon or silicon oxide with the thickness of dozens to hundreds of nanometers as a soft X-ray passing window; below this thickness window, the three materials have proven to be able to withstand pressures above 1 atmosphere; the high transmittance of the soft X-ray in the wave band of 100-2000eV can be ensured through the complementation of the three materials, so that a strong spectral signal is obtained.
Drawings
FIG. 1 is a schematic structural diagram of a dynamic in-situ gas-phase reaction cell that can be used for soft X-ray spectroscopy experiments according to the present invention;
FIG. 2 is an exploded view of a main body of a dynamic in-situ gas phase reaction cell for soft X-ray spectroscopy;
FIG. 3 is an exploded view of a support member of a dynamic in-situ gas phase reaction cell for soft X-ray spectroscopy;
FIG. 4 is an exploded view of the external connection components in a dynamic in-situ gas phase reaction cell for soft X-ray spectroscopy;
FIG. 5 is a schematic structural diagram of a reaction cell cover in a dynamic in-situ gas phase reaction cell for soft X-ray spectroscopy experiments according to the present invention;
FIG. 6 is a schematic structural diagram of a metal partition plate in a dynamic in-situ gas-phase reaction cell for soft X-ray spectroscopy experiments according to the present invention;
FIG. 7 is a schematic structural diagram of a sample holder in a dynamic in-situ gas-phase reaction cell for soft X-ray spectroscopy;
FIG. 8 is a graph of the light transmittance of 100-2000eV energy X-rays in different window materials.
Detailed Description
Referring to fig. 1 to 7, the present invention provides a dynamic in-situ gas phase reaction tank for soft X-ray spectroscopy experiments, comprising a reaction tank main body 1, a reaction tank support member 2, and an external connection member 3; wherein:
the reaction tank main body 1 is provided with a sample cavity for placing a sample and a first light through hole 111 communicated with the sample cavity, a metal partition 14 is arranged in the sample cavity, a second light through hole 141 communicated with the first light through hole 111 is arranged on the metal partition 14, and a light through window 16 matched with the second light through hole 141 is arranged on the inner side of the metal partition 14.
The reaction cell support 2 includes a support pipe connected to the reaction cell main body 1.
The external connecting piece 3 comprises a connector, a differential pumping pipeline 33, two gas pipelines 38, an electronic yield signal line 35 and a bias line 36, the connector is connected with one end of the supporting pipe far away from the reaction tank main body 1, the differential pumping pipeline 33 is connected with the connector, the differential pumping pipeline 33 is provided with a vacuum interface for connecting a vacuum pump, and one ends of the two gas pipelines 38 and the electronic yield signal line 35 sequentially penetrate through the connector and the supporting pipe to be connected with the reaction tank; one end of the bias line 36 passes through the differential pumping pipeline 33, the connector, the support pipe, the reaction tank main body 1 and is connected with the metal partition 14 in sequence.
The reaction tank provided by the invention adopts the metal partition plate 14 to apply bias voltage, so that an electric field is generated between the sample and the metal partition plate 14, ionized gas particles are pulled away from the surface of the sample, the background noise is reduced, and the collection of an electron yield signal is possible.
Referring to fig. 2, in the present embodiment, the reaction cell main body 1 includes a reaction cell cover 11, an insulating sleeve 13, and a reaction cell base 12; wherein:
the reaction tank cover 11 is made of polyetheretherketone material, and can also be made of machinable materials such as alumina ceramics, boron nitride, mica and polyimide. Referring to FIG. 5, the reaction cell cover 11 is provided with a mounting hole 112 and a first light passing hole 111 communicating with the mounting hole 112, and the opening angle of the first light passing hole 111 is 120 deg. for increasing the incidence and acceptance angles of light.
The insulating sleeve 13 is made of polyetheretherketone material, and can also be made of machinable materials such as alumina ceramics, boron nitride, mica, polyimide, and the like. Insulating sleeve 13 sets up in the mounting hole and is located metal partition 14 and keeps away from first smooth through-hole 111 one side, and insulating sleeve 13 external diameter is the same with mounting hole 112 diameter and its height is the same with the mounting hole degree of depth, and the insulating sleeve 13 both ends outside is equipped with 0.5mm chamfer to make things convenient for insulating sleeve 12 to install, insulating sleeve 12 lateral wall is opened has the degree of depth that supplies the bias voltage line to pass through, the width is 1 mm's groove. The insulating sleeve 13 is provided with a sample cavity, a sample support 15 for placing a sample a is arranged in the sample cavity, and the sample support 15 is made of oxygen-free copper and is plated with 100-nanometer gold on the surface. As shown in fig. 7, the center of the sample holder 15 is provided with a central circular groove 151 for placing a powder sample a, the depth of the central circular groove 151 is 0.5mm, the sample a is generally powder, the powder is pressed into a cylinder with the diameter of 1-3mm and the thickness of 0.5mm by a tablet press and a die, the cylinder is placed in the central circular groove 151, the sample a can have other properties which can be placed in the sample holder 15, and the shape of the sample holder 15 can be correspondingly modified; the sample holder 15 is provided with gas channels 152 for gas pipelines to pass through on two sides of the central circular groove 151, and the sample holder 15 is also provided with a communicating groove 153 for communicating the central circular groove 151 with the gas channels 152.
The reaction tank provided by the invention improves the light intensity reaching the sample surface by reducing the distance between the window and the sample a, improves the signal intensity, and achieves a reasonable Reynolds coefficient by introducing gas through the gas pipeline 38 and adjusting the flow rate of the gas, thereby ensuring a faster gas renewal speed on the surface of the material; the center of the sample holder 15 is provided with a communicating groove for communicating the central circular groove with the gas channel, so that gas can smoothly flow through the communicating groove to avoid forming turbulence, therefore, the gas updating efficiency is high, and the change of the material and the gas interface can be observed conveniently.
The reaction chamber base 12 is connected with the reaction chamber cover 11 through screws for sealing the sample chamber, and the material thereof is 316 stainless steel. One side of the reaction cell substrate 12, which is close to the insulating sleeve 13, is provided with a first pillar which extends into the sample cavity and is used for bearing the sample holder 15, and the surface of the first pillar is plated with 100 nm gold. The connecting surface of the reaction tank base 12 and the reaction tank cover 11 is provided with an annular groove with the depth of 1.6mm, the annular groove is used for placing a first sealing ring, the first sealing ring is made of fluororubber or silicon rubber, and the inner diameter is slightly larger than the outer diameter of the insulating sleeve 13. A first round hole for a step-shaped threaded hole for connecting a gas pipeline and a bias line to penetrate is formed in the annular groove close to the first pillar, and a second round hole for guiding the gas pipeline into a sample support plane is formed in one side, close to the sample support, of the step-shaped threaded hole.
Referring to fig. 6, in this embodiment, the metal partition 14 is made of 316 stainless steel, a second pillar 142 is disposed on one side of the metal partition 14 close to the insulating sleeve 13, and a second light through hole 141 with an opening angle of 120 ° is disposed on the metal partition 14 for matching with the first light through hole 111 to increase the incident and receiving angles of light. The third sealing ring 110 is arranged on the connecting surface of the metal partition plate 14 and the reaction tank cover 11.
In this embodiment, the substrate of the light-transmitting window 16 is a cuboid, the external length and width are both 10mm, the thickness is 0.5mm or 0.2mm, a small window is arranged in the middle of the substrate, the length and width are generally 0.5mm × 1mm or 1mm × 1mm, the thickness of the window is dozens of nanometers to hundreds of nanometers, the thickness of the window is generally 100 nanometers, the material of the light-transmitting window 16 can be adjusted according to the experimental requirements, and can be silicon nitride, silicon oxide or carbon, and the pressure resistance intensity of the light-transmitting window 16 is not lower than 1 atmosphere. An annular insulating gasket 17 with a gap is arranged between the light-transmitting window 16 and the metal partition plate 14, the insulating gasket 17 is made of polyimide, and a second sealing ring 19 is arranged on the connecting surface of the insulating gasket 17 and the metal partition plate 14.
In this embodiment, 100 nm thick silicon nitride, carbon or silicon oxide is used as the soft X-ray passing window, and the light transmittance curve is shown in fig. 8, the three materials have been proved to be able to withstand a pressure of 1 atm or more under the thickness of the window, and the high transmittance of the soft X-ray in the wavelength band of 100-2000eV can be ensured by the complementation of the three materials, so as to obtain a strong spectrum signal.
Referring to fig. 3, in the present embodiment, the support pipe includes an adjustment connection pipe 21 and an insulation connection pipe 22, in which:
the adjusting connecting pipe 21 is a cylindrical pipe made of stainless steel and has the model number of 304, and the length of the adjusting connecting pipe 21 can be adjusted according to the size of a cavity of the experimental system. The two ends of the adjusting connecting pipe 21 are respectively connected with a first connecting cover 23 and a second connecting cover 24, the first connecting cover 23 is provided with a first through hole through which the bias line 36 passes, and the second connecting cover 24 is provided with a second through hole through which the bias line 36 passes. The first connecting cover 23 is a stepped cylinder, the material is 304 stainless steel, the outer diameter of a larger cylinder of the first connecting cover is the same as the outer diameter of the adjusting connecting pipe, the outer diameter of a smaller cylinder of the first connecting cover is the same as the inner diameter of the adjusting connecting pipe, an annular groove is formed in the stepped surface of the larger diameter of the first connecting cover, an O-shaped rubber ring or vacuum rubber can be placed as required for sealing, and the center of the first connecting cover 23 is a first through hole for the air passage pipeline, the electronic yield signal line 35 and the bias line 36 to pass through. The second connecting cover 24 is a flange and is welded with the adjusting connecting pipe 21, the second connecting cover is a stepped cylinder, the material is 304 stainless steel, the middle part is provided with a second through hole, the diameter of the second through hole is the same as the inner diameter of the adjusting connecting pipe and is used for a gas path pipeline, an electronic yield signal line 35 and a bias line 36 to pass through, the top of the second connecting cover 24 is a circular groove, the diameter of the circular groove is 0.5mm deep, the diameter of the circular groove is the same as the outer diameter of the adjusting connecting pipe, and the outer ring of the top of the second connecting cover 24 is a 2mm chamfer.
The insulating connection tube 22 is a tapered hexagonal prism made of polyetheretherketone, or a processable material such as alumina ceramic, boron nitride, mica, polyimide, etc. One end of the insulating connecting pipe 22 is connected with the reaction tank substrate 12 through a screw, the other end of the insulating connecting pipe is connected with the first connecting cover 23 through a screw, and a fifth sealing ring is arranged on the connecting surface of the reaction tank substrate 12 and the insulating connecting pipe 22. The middle part of the insulating connecting pipe 22 is a circular through hole for the air channel pipeline and the lead to pass through, and the inner side of the through hole is provided with a 0.5mm chamfer so as to facilitate the smooth passing of the air channel pipeline and the lead.
Referring to fig. 4, in the present embodiment, the connectors include a main connector 31, a signal line connector 32, a bias line connector 34 and two gas pipe connectors 37, and the differential pumping pipe 33, the signal line connector 32 and the two gas pipe connectors 37 are all connected to the main connector 31. Wherein:
the main body of the gas pipeline connector 37 is a screw assembly of a CF16 flange and a central through hole which are specially designed, the CF16 flange which is specially designed is a step cylinder made of 304 stainless steel, the large-diameter cylinder is a standard CF16 flange, the center of the small-diameter cylinder is a threaded through hole, the small-diameter cylinder is matched with a screw of the central through hole, and a gas pipeline can pass through the central through hole of the screw.
The signal line connector 32 is used for connecting with an electronic yield signal line and leading out an electronic signal, and is a standard BNC type interface based on a CF16 flange, and the main material is 304 stainless steel and alumina ceramic.
The bias line connector 34 is a standard electrical connector based on a CF16 flange, the main materials are 304 stainless steel and alumina ceramics, and the three electrical interfaces are total, wherein one of the three electrical interfaces is used for being connected with a bias line and leading out to an external power supply to apply voltage to a metal partition plate, and the other two electrical interfaces are standby and can be used for connecting a lead when the function of the reaction tank is upgraded, such as the additional electrochemical function.
Referring to fig. 4, in this embodiment, the main connector 31 is provided with 1 CF35 flange opening 311 and 5 CF16 flange openings 312, the main connector 31 is connected to the second connection cover 24 through the CF35 flange opening 311, and a fourth sealing ring 39 is provided on a connection surface between the CF35 flange opening 311 and the second connection cover 24;
wherein 3 CF16 flange openings 312 are uniformly distributed on the back along the circumference of the CF35 flange opening 311, the included angle between the 3 CF16 flange openings 312 and the knife edge flange face of the CF35 flange opening 311 is 30 degrees, and the signal connector and the two gas pipeline connectors 37 are both CF16 flanges and are respectively connected with the 3 CF16 flange openings 312;
the other CF16 flange port 312 and the CF35 flange port 311 are directly communicated, the included angle between the CF16 flange port 312 and the CF35 flange port 311 is 180 degrees, and the differential pumping pipeline 33 is connected with the CF16 flange port 312;
in this embodiment, the main connector 31 is further provided with a spare CF16 flange port 312 in a sealed state, the spare CF16 flange port 312 is made of 304 stainless steel, a standard CF16 flange blind plate is connected, and the spare CF16 flange port 312 can be replaced by other connectors to meet the requirement of increasing the functions of the reaction tank.
In this embodiment, the core wire of the electronic yield signal line 35 is made of silver-plated aluminum wire, and the outer portion of the electronic yield signal line is wrapped by an insulation shielding structure formed by a polyimide film and a stainless steel mesh, so as to reduce the interference of external signals, and one end of the electronic yield signal line 35 sequentially passes through the signal line connector 32, the main connector 31, the second connection cover 24, the adjusting connection pipe 21, the first connection cover 23, and the insulation connection pipe 22 and then is connected and conducted with the reaction tank substrate 12 through stainless steel screws.
In this embodiment, after passing through the gas pipe connector 37, the main connector 31, the second connecting cover 24, the adjusting connecting pipe 21, and the first connecting cover 23 in sequence, one end of each of the two gas pipes 38 is in threaded connection with the reaction cell base 12 by using a hollow screw 381 and a rubber seal 382 and is communicated with the sample chamber, and the hollow screw 381 is made of polyether ether ketone.
In this embodiment, the differential pumping pipeline 33 is a CF16 tee pipeline made of 304 stainless steel, the first port of the differential pumping pipeline 33 is connected to the CF16 flange port 312, the second port is connected to the bias line connector 34, the third port is a vacuum port for connecting a vacuum pump, and the vacuum inside the reaction tank is maintained by differential pumping of the vacuum pump.
In this embodiment, the bias line connector 34 is connected to one end of the differential pumping pipeline 33, which is far from the main connector, and one end of the bias line 36 sequentially passes through the bias line connector 34, the differential pumping pipeline 33, the main connector 31, the second connecting cover 24, the adjusting connecting pipe 21, the first connecting cover 23, the insulating connecting pipe 22, the reaction tank substrate 12 and the metal partition 14 to be connected.
The invention is insulated by materials such as polyether-ether-ketone, polyimide, alumina ceramics and the like; sealing is carried out by materials such as a rubber sealing ring and an oxygen-free copper gasket and by modes such as plane pressing and seamless welding; the mechanical strength of the reaction tank is provided by stainless steel, polyether-ether-ketone and other materials; gas transmission is carried out through gas path pipelines made of materials such as polyether-ether-ketone, stainless steel, copper and the like; background noise is reduced and signal intensity is improved in a mode of applying bias voltage to the metal partition plate; experimental errors caused by reaction of structural materials of the reaction tank and gas are eliminated in a manner of plating gold on the reaction tank and the sample holder; the signal purity is improved in a metal mesh shielding wire mode; realizing soft X-ray transmission by means of material windows such as silicon nitride, silicon oxide, carbon and the like; the pressure required for sealing is provided by means of screw tightening.
The reaction cell of the present embodiment employs the reaction cell main body 1, the reaction cell support 2, and the external connection member 3, which are separated from each other, in order to facilitate the maintenance of parts and the replacement of samples by modularization, and the number of parts can be reduced by an integrated design while maintaining most functions.
The connecting screw used in the reaction tank of this embodiment is made of 316 stainless steel, and the material of the screw can be replaced by other metal materials such as copper, aluminum, titanium alloy, and the like, and insulating materials such as polyetheretherketone, boron nitride, alumina, and the like, so that the strength is reduced, but the structure of the reaction tank can still be maintained.
The sealing ring material used in the reaction cell of this embodiment may be replaced by a compressible sealing material such as polytetrafluoroethylene, in addition to fluororubber and silicone rubber.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A dynamic in-situ gas phase reaction tank for soft X-ray spectroscopy experiments is characterized by comprising a reaction tank main body (1), a reaction tank supporting piece (2) and an external connecting piece (3); the reaction tank main body (1) is provided with a sample cavity for placing a sample and a first light through hole (111) communicated with the sample cavity, a metal partition plate (14) is arranged in the sample cavity, a second light through hole (141) communicated with the first light through hole (111) is arranged on the metal partition plate (14), and a light through window (16) matched with the second light through hole (141) is arranged on the inner side of the metal partition plate (14); the reaction tank support piece (2) comprises a support pipe, and the support pipe is connected with the reaction tank main body (1); the external connecting piece (3) comprises a connector, a differential pumping pipeline (33), an electronic yield signal line (35) and a bias line (36), the connector is connected with one end of the supporting pipe, which is far away from the reaction tank main body (1), the differential pumping pipeline (33) is connected with the connector, the differential pumping pipeline (33) is provided with a vacuum interface for connecting a vacuum pump, and one end of the electronic yield signal line (35) sequentially penetrates through the connector and the supporting pipe to be connected with the reaction tank; one end of a bias line (36) sequentially penetrates through the differential pumping pipeline (33), the connector, the support pipe and the reaction tank main body (1) to be connected with the metal partition plate (14);
the reaction tank main body (1) comprises a reaction tank cover (11), an insulating sleeve (13), a metal partition plate (14) and a reaction tank base (12), the reaction tank cover (11) is provided with a mounting hole and a first light through hole (111) communicated with the mounting hole, the insulating sleeve (13) and the metal partition plate (14) are arranged in the mounting hole, the metal partition plate (14) is positioned on one side, close to the light through hole, of the insulating sleeve (13), the insulating sleeve (13) is provided with a sample cavity, and a sample support (15) for placing a sample is arranged in the sample cavity; the reaction cell base (12) is connected with the reaction cell cover (11) for sealing the sample cavity.
2. The dynamic in-situ gas-phase reaction cell for soft X-ray spectroscopy experiments according to claim 1, wherein the reaction cell cover (11) and the insulating sleeve (13) are made of polyetheretherketone material.
3. The dynamic in-situ gas phase reaction cell for soft X-ray spectroscopy experiments according to claim 1, wherein the side of the reaction cell base (12) near the insulating sleeve (13) is provided with a first pillar extending into the sample cavity and used for carrying the sample holder (15); a first sealing ring is arranged on the connecting surface of the reaction tank base (12) and the reaction tank cover (11).
4. The dynamic in-situ gas phase reaction cell for the soft X-ray spectroscopy experiment of claim 1, wherein a second pillar is arranged on one side of the metal partition plate (14) close to the insulating sleeve (13), an annular insulating gasket (17) with a gap is arranged between the light transmission window (16) and the metal partition plate (14), and a second sealing ring (19) is arranged on the connecting surface of the insulating gasket (17) and the metal partition plate (14); a third sealing ring (110) is arranged on the connecting surface of the metal clapboard (14) and the reaction tank cover (11).
5. The dynamic in-situ gas-phase reaction cell applicable to the soft X-ray spectroscopy experiment of any one of claims 1 to 4, wherein the diameters of the first optical through hole (111) and the second optical through hole (141) are gradually reduced from outside to inside, and the aperture angles of the first optical through hole (111) and the second optical through hole (141) are both 120 °.
6. The dynamic in-situ gas phase reaction tank for the soft X-ray spectroscopy experiment as claimed in any one of claims 2 to 4, wherein the supporting tube comprises an adjusting connecting tube (21) and an insulating connecting tube (22), the length of the adjusting connecting tube (21) is adjustable, two ends of the adjusting connecting tube (21) are respectively connected with a first connecting cover (23) and a second connecting cover (24), the first connecting cover (23) is provided with a first through hole through which the bias line (36) passes, and the second connecting cover (24) is provided with a second through hole through which the bias line (36) passes; one end of the insulating connecting pipe (22) is connected with the reaction tank substrate (12) through a screw, and the other end of the insulating connecting pipe is connected with the first connecting cover (23) through a screw; the insulating connecting pipe (22) is made of polyether-ether-ketone material.
7. The dynamic in-situ gas-phase reaction cell for the soft X-ray spectroscopy experiment of claim 6, wherein the external connector (3) further comprises two gas pipelines (38), the connectors comprise a main connector (31), a signal line connector (32), a bias line connector (34) and two gas pipeline connectors (37), and the differential pumping pipeline (33), the signal line connector (32) and the two gas pipeline connectors (37) are all connected with the main connector (31); one end of an electronic yield signal wire (35) sequentially penetrates through a signal wire connector (32), a main connector (31), a second connecting cover (24), an adjusting connecting pipe (21), a first connecting cover (23) and an insulating connecting pipe (22) to be connected and communicated with the reaction cell substrate (12), and one ends of two gas pipelines (38) sequentially penetrate through a gas pipeline connector (37), the main connector (31), the second connecting cover (24), the adjusting connecting pipe (21) and the first connecting cover (23) to be in threaded connection with the reaction cell substrate (12) and communicated with the sample cavity; the bias line joint (34) is connected with one end, far away from the main connector, of the differential pumping pipeline (33), one end of the bias line (36) sequentially penetrates through the bias line joint (34), the differential pumping pipeline (33), the main connector (31), the second connecting cover (24), the adjusting connecting pipe (21), the first connecting cover (23), the insulating connecting pipe (22) and the reaction tank substrate (12) to be connected with the metal partition plate (14).
8. The dynamic in-situ gas phase reaction cell for soft X-ray spectroscopy experiments as claimed in claim 7, wherein the general connection head (31) is provided with 1 CF35 flange port (311) and 5 CF16 flange ports (312), and the general connection head (31) is welded with the second connection cover (24) through the CF35 flange port (311); wherein 3 CF16 flange mouths (312) are uniformly distributed on the back surface along the circumference of the CF35 flange mouth (311), the included angle between the 3 CF16 flange mouths (312) and the knife edge flange surface of the CF35 flange mouth (311) is 30 degrees, and a signal connector and two gas pipeline connectors (37) are manufactured on the basis of the CF16 flange and are respectively connected with the 3 CF16 flange mouths (312); the other CF16 flange port (312) and the CF35 flange port (311) are communicated in a straight way, the included angle between the CF16 flange port (312) and the edge flange face of the CF35 flange port (311) is 180 degrees, and a differential pumping pipeline (33) is connected with the CF16 flange port (312); the other CF16 flange port (312) is a spare CF16 flange port in a sealed state; and a fourth sealing ring (39) is arranged on the connecting surface of the CF35 flange opening (311) and the second connecting cover (24).
9. The dynamic in-situ gas-phase reaction cell applicable to the soft X-ray spectroscopy experiment of claim 8, wherein the differential pumping pipeline (33) is a CF16 tee pipeline, the bias line connector (34) is a CF16 flange, a first passage of the differential pumping pipeline (33) is connected with a CF16 flange port (312), a second passage is connected with the bias line connector (34), and a third passage is a vacuum port for connecting a vacuum pump.
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| CN112083048B (en) * | 2020-09-15 | 2021-12-14 | 中国科学技术大学 | Dynamic in-situ liquid phase reaction tank for electrochemical test |
| CN112083020B (en) * | 2020-09-16 | 2021-10-19 | 中国科学技术大学 | Vacuum system for in-situ soft X-ray absorption spectroscopy experiment |
| CN113125479A (en) * | 2021-04-15 | 2021-07-16 | 中国科学技术大学 | Reaction device for in-situ temperature-changing X-ray scattering characterization |
| CN113566448A (en) * | 2021-07-13 | 2021-10-29 | 中国科学院上海微系统与信息技术研究所 | Cooling device for soft X-ray spectroscopy test |
| CN114486736B (en) * | 2022-01-10 | 2023-10-10 | 山东大学 | Multifunctional spectrum and X-ray diffraction in-situ reaction chamber and application |
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