CN112083020B - Vacuum system for in-situ soft X-ray absorption spectroscopy experiment - Google Patents

Vacuum system for in-situ soft X-ray absorption spectroscopy experiment Download PDF

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CN112083020B
CN112083020B CN202010972924.3A CN202010972924A CN112083020B CN 112083020 B CN112083020 B CN 112083020B CN 202010972924 A CN202010972924 A CN 202010972924A CN 112083020 B CN112083020 B CN 112083020B
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vacuum
pipeline
assembly
unthreaded hole
way
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CN112083020A (en
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李鑫
冯雪飞
梁立军
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University of Science and Technology of China USTC
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University of Science and Technology of China USTC
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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
    • G01N23/06—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 and measuring the absorption
    • G01N23/083—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 and measuring the absorption the radiation being X-rays

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Abstract

The invention discloses a vacuum system for in-situ soft X-ray absorption spectroscopy experiments, which comprises a secondary differential pumping assembly, a diaphragm assembly, a gold mesh aperture assembly, a primary differential pumping assembly and an experimental station, wherein the secondary differential pumping assembly, the diaphragm assembly, the gold mesh aperture assembly, the primary differential pumping assembly and the experimental station are sequentially connected from a light source to an emergent direction through a vacuum pipeline; the gold mesh unthreaded hole assembly comprises a reflecting mirror and an unthreaded hole plate body, wherein the reflecting mirror is provided with an oblique section with a through hole in the middle, and the oblique section is opposite to a window of an observation port on the experiment station; the middle part of the unthreaded hole plate body is provided with an unthreaded hole, and the diameter of the unthreaded hole is 2mm-6 mm. In the vacuum system that can be used to soft X ray absorption spectroscopy of normal position experiment that this application provided, the diameter of unthreaded hole is 2mm-6mm, reduces the unthreaded hole diameter, reduces the conductance, and adopts speculum through-hole and unthreaded hole constitution dual-optical-hole structure, prolongs the time that gas, liquid sample got into the beam line pipeline, thereby in time closes for the valve provides sufficient time to respond, and then reduces and cause the damage to front end optical device.

Description

Vacuum system for in-situ soft X-ray absorption spectroscopy experiment
Technical Field
The invention relates to the technical field of in-situ experiments, in particular to a vacuum system for in-situ soft X-ray absorption spectroscopy experiments.
Background
In the field of scientific research, the in-situ experimental technology refers to a technology for observing physical and chemical changes of substances in real time in a simulated real environment or in a device working state. Compared with the traditional ex-situ experiment technology, the in-situ experiment process does not change the existing state of the reaction substance, and simultaneously can track and observe the continuous change of the substances at different time nodes. By applying the method, scientists study the intermediate processes such as catalytic reaction, crystal growth, biological evolution and the like, thereby understanding the deep mechanism of various natural phenomena.
Among various detection methods adopted by the in-situ experiment technology, the soft X-ray absorption spectroscopy takes X-rays with continuously adjustable energy as an excitation light source, characterizes the electronic structure of an experimental object, has the characteristics of element resolution, scannable unoccupied state and the like, and plays an important role in the research fields of energy, environment, materials and the like. However, the existing soft X-ray absorption spectroscopy experimental system often needs to consider the compatibility problem of solid sample detection, and the design cannot completely meet the requirements of in-situ experiments, such as: when the traditional soft X-ray absorption spectroscopy experiment station is connected with an ultrahigh vacuum light beam line, when the in-situ reaction device is arranged in a vacuum system, if a window at the front end of the device is broken, the air pressure of a cavity is suddenly increased, the whole light beam line, particularly an optical device, can be damaged, and the electronic storage ring can be polluted when the air pressure is serious.
Therefore, how to reduce the damage to the optical device is an urgent technical problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a vacuum system for in-situ soft X-ray absorption spectroscopy experiments, which can reduce damage to optical devices.
In order to achieve the aim, the invention provides a vacuum system for in-situ soft X-ray absorption spectroscopy experiments, which comprises a secondary differential pumping assembly, a diaphragm assembly, a gold mesh aperture assembly, a primary differential pumping assembly and an experiment station, wherein the secondary differential pumping assembly, the diaphragm assembly, the gold mesh aperture assembly, the primary differential pumping assembly and the experiment station are sequentially connected from a light source to an emergent direction through a vacuum pipeline;
the gold mesh light hole assembly comprises:
the reflecting mirror is provided with an oblique cutting plane with a through hole in the middle, and the oblique cutting plane is opposite to a window of an observation port on the experiment station;
and the light hole plate body is provided with a light hole in the middle, and the diameter of the light hole is 2-6 mm.
Preferably, the laboratory station comprises:
the X-Y moving platform is used for mounting the in-situ experiment device, a mounting opening of the X-Y moving platform can be adjusted along the direction vertical to the ground and parallel to the ground, and the mounting opening of the X-Y moving platform is over against the X-ray light source;
a vacuum chamber assembly for mounting a probe and apparatus associated with an in situ experimental setup thereof, said vacuum chamber assembly comprising:
the vacuum cavity shell is connected with the XY moving platform;
the fast valve sensor is arranged on the vacuum cavity shell and is used for detecting the vacuum degree in the cavity of the vacuum cavity shell;
the secondary differential pumping assembly comprises a vacuum fast valve for closing and communicating a vacuum pipeline between a vacuum cavity where an optical device at the front end of the secondary differential pumping assembly is located and the secondary differential pumping assembly, the vacuum fast valve is connected with the fast valve sensor, and when the experiment station runs, the vacuum fast valve is in an open state, so that X rays can be incident to the experiment station; when the fast valve sensor detects that the air pressure in the vacuum cavity is higher than a set value or is manually closed, the vacuum fast valve is closed within 40 ms.
Preferably, the laboratory station further comprises a first vacuum gauge mounted on the vacuum chamber housing, the first vacuum gauge being configured to read a vacuum level in a chamber of the vacuum chamber housing;
the first-stage differential pumping assembly comprises:
a first port of the first three-way connecting pipeline is connected with the vacuum cavity shell;
the first pneumatic gate valve is used for closing and communicating a vacuum pipeline between the primary differential pumping assembly and the gold mesh unthreaded hole assembly and is connected with a second interface of the first three-way connecting pipeline;
the second pneumatic gate valve is connected with a third interface of the first tee connecting pipeline;
the second pneumatic gate valve is used for closing and communicating a vacuum pipeline between the first tee joint connecting pipeline and the first turbo molecular pump;
the second-stage differential pumping assembly further comprises:
a first interface of the second three-way connecting pipeline is connected with the diaphragm assembly, and a second interface of the second three-way connecting pipeline is connected with the vacuum fast valve;
the third port of the second three-way connecting pipeline is connected with the third pneumatic gate valve;
and the third pneumatic gate valve is used for closing and communicating the second tee joint connecting pipeline and the second turbo molecular pump.
Preferably, the inner diameters of the air exhaust pipeline of the first-stage differential pumping assembly and the air exhaust pipeline of the second-stage differential pumping assembly are both 45mm-55 mm.
Preferably, the laboratory station further comprises:
the fourth pneumatic gate valve is opened when the inner cavity of the vacuum cavity shell needs to be vacuumized by an auxiliary pump, so that the air pumping process is accelerated;
and the fourth pneumatic gate valve is used for separating or communicating the third turbo molecular pump and the inner cavity of the vacuum cavity shell.
Preferably, the laboratory station further comprises:
a chamber support for supporting the vacuum chamber housing;
the six-axis adjusting device is used for adjusting the axial displacement and the rotation angle of the vacuum cavity shell;
the six-axis adjusting device is installed on the base.
Preferably, the six-axis adjusting device comprises six independently adjustable moving rods, each moving rod comprises a pipe body with an internal thread in the middle section and joint nuts positioned at two ends of the pipe body, and two ends of each moving rod are respectively connected with the cavity support and the base through screws;
six the removal stick is two respectively and is used for adjusting vacuum chamber shell horizontal position's first removal stick and four second removal sticks that are used for adjusting vacuum chamber shell height and rotation angle.
Preferably, the gold mesh aperture assembly further comprises:
the gold mesh fixing rod is a rotating shaft fixed in the center of the flange, the gold mesh is fixed at the front end of the rotating shaft, and the gold mesh is positioned on an X-ray light path in a working state;
the gold mesh current reading port is an electrode fixed in the center of the flange, and the electrode is connected with a gold mesh at the front end of the gold mesh fixing rod and insulated from an external pipeline;
the welding corrugated pipe is used for connecting an external pipeline of the gold mesh aperture assembly and the diaphragm assembly;
the front end interface of the first six-way pipeline is connected with the welding corrugated pipe along the direction of the light path and is used for being communicated to the diaphragm assembly; a first window is arranged at the upper end interface of the first six-way pipeline; a second window is arranged at the left end interface of the first six-way pipeline; the right end interface of the first six-way pipeline is connected with the gold mesh fixing rod;
the rear end interface of the first six-way pipeline is connected with the first interface of the third three-way connecting pipeline to form a closed space required for maintaining the pipeline, the gold mesh and the pipeline where the unthreaded plate body is located are communicated, and the upper end of the third three-way connecting pipeline forms a second interface for installing a window;
the middle part of the hollow manual valve is provided with a through hole for installing a unthreaded hole plate body, the rear end of the third three-way connecting pipeline is provided with a third interface along the direction of a light path to be connected with the hollow manual valve, and the upper part of the hollow manual valve is provided with a handle which can be used for arranging the unthreaded hole of the unthreaded hole plate in the center of the light path or moving out the unthreaded hole of the unthreaded hole plate through rotation;
moving the rod;
the gold evaporation source is a crucible connected with double electrodes, gold particles are placed in the middle of the crucible and used for carrying out in-situ gold film plating on a gold net, and a lower end interface of the first six-way pipeline is connected with the gold evaporation source;
the supporting frame comprises an upper plate and a lower plate, the upper plate is used for installing a vacuum pipeline of the gold mesh unthreaded hole assembly, the lower plate is connected with the ground, and the moving rod is used for adjusting the height and the horizontal rotation angle of the upper plate.
Preferably, the diaphragm assembly comprises:
the number of the adjustable square diaphragms is two, and the two adjustable square diaphragms are respectively horizontally and vertically arranged;
the electric control linear driver is used for adjusting the position of the adjustable square aperture in the vertical direction;
the manual linear driver is used for adjusting the relative position of the adjustable square aperture and the optical path in the horizontal direction;
the two second six-way pipelines are connected to form a vacuum pipeline, the upper end interface of the first second six-way pipeline in the optical path direction is connected with an electric control linear driver, and the front end interface of the first second six-way pipeline is provided with a corrugated pipe and is connected with the secondary differential pumping assembly through a pipeline with adjustable length; the upper end interface of the second six-way pipeline is connected with a window, the left end interface of the second six-way pipeline is connected with the manual linear driver, and blind plates are detachably mounted on other interfaces of the second six-way pipeline for standby;
the second vacuum gauge pipe is used for measuring the vacuum degree of the inner cavity of the diaphragm assembly, and the right end interface of the first six-way pipe is connected with the second vacuum gauge pipe.
Preferably, the inner diameter of the pumping ports of the first turbo molecular pump, the second turbo molecular pump and the third turbo molecular pump is 55mm to 65 mm.
In the technical scheme, the vacuum system for the in-situ soft X-ray absorption spectroscopy experiment comprises a secondary differential pumping assembly, a diaphragm assembly, a gold mesh aperture assembly, a primary differential pumping assembly and an experiment station which are sequentially connected from a light source to an emergent direction through a vacuum pipeline.
The gold net unthreaded hole subassembly includes speculum and unthreaded hole plate body, and the speculum is equipped with the scarf that the middle part was equipped with the through-hole, and the scarf just right with the window of observing the mouth on the laboratory bench. The middle part of the unthreaded hole plate body is provided with an unthreaded hole, and the diameter of the unthreaded hole is 2mm-6 mm.
According to the above description, in the vacuum system for in-situ soft X-ray absorption spectroscopy experiments provided by the application, the diameter of the optical hole is 2mm-6mm, the diameter of the optical hole is reduced, the conductance is reduced, and the reflector adopts the reflector through hole and the optical hole to form a double-optical-hole structure, so that the time for gas and liquid samples to enter the optical beam line pipeline is prolonged, enough time is provided for the valve to respond, and therefore the valve is closed in time, and further damage to the front-end optical device is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a vacuum system that can be used for in-situ soft X-ray absorption spectroscopy experiments according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a laboratory station according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a vacuum chamber assembly according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a first-stage differential pumping assembly according to an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a gold mesh aperture component according to an embodiment of the present invention;
FIG. 6 is a structural position diagram of a dual optical aperture inside a pipe of a gold mesh optical aperture assembly according to an embodiment of the present invention;
FIG. 7 is a schematic structural diagram of a diaphragm assembly provided in an embodiment of the present invention;
FIG. 8 is a schematic structural diagram of an adjustable square aperture provided in an embodiment of the present invention;
fig. 9 is a schematic structural diagram of a two-stage differential pumping assembly according to an embodiment of the present invention.
Wherein in FIGS. 1-9:
A. an experimental station; a-1, an XY moving platform;
a-2, a vacuum cavity component; a-2-1, a first observation port; a-2-2 and a second observation port; a-2-3, a third observation port; a-2-4, a detector mounting port; a-2-5, an X-ray source inlet; a-2-6, a detector mounting port; a-2-7, a spare air pumping system mounting port; a-2-8, spare detector mounting port; a-2-9, a quick valve sensor mounting port; a-2-10, a fast valve sensor; a-2-11, a first vacuum gauge; a-2-12, a fourth pneumatic gate valve; a-2-13, a third turbomolecular pump;
a-3, a cavity support; a-4, a six-axis adjusting device; a-5, a base;
B. a first-stage differential pumping assembly; b-1, connecting a first tee joint with a pipeline; b-2, a first pneumatic gate valve; b-3, a second pneumatic gate valve; b-4, a first turbo molecular pump; b-5, a pipeline bracket;
C. a gold mesh aperture assembly; c-1, fixing a gold net rod; c-2, a gold net current reading port; c-3, welding the corrugated pipe; c-4, a first six-way pipeline; c-5, connecting a third tee joint with a pipeline; c-6, a hollow manual valve; c-7, moving the rod; c-8, gold evaporation source; c-9, a support frame; c-10, a reflector; c-11, a unthreaded hole plate body;
D. a diaphragm assembly;
d-1, adjusting the square aperture; d-1-1, a telescopic rod; d-1-2, an aperture upper layer adjusting plate; d-1-3, diaphragm fixing flange; d-1-4, an aperture lower layer adjusting plate; d-1-5, step sliding blocks;
d-2, an electrically controlled linear driver; d-3, manual linear drive; d-4, a second six-way pipeline; d-5, a second vacuum gauge; d-6, a bottom support frame;
E. a second-stage differential pumping assembly; e-1, a vacuum quick valve; e-2, connecting a second tee joint with a pipeline; e-3, a third pneumatic gate valve; e-4, a second turbomolecular pump; e-5, a pipeline bracket.
Detailed Description
The core of the invention is to provide a vacuum system for in-situ soft X-ray absorption spectroscopy experiments, which can reduce the damage to optical devices.
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and embodiments.
Please refer to fig. 1 to fig. 9.
In a specific implementation manner, the vacuum system for in-situ soft X-ray absorption spectroscopy experiments provided by the specific embodiment of the present invention includes a second-stage differential pumping assembly E, a diaphragm assembly D, a gold mesh aperture assembly C, a first-stage differential pumping assembly B, and an experiment station a, which are sequentially connected through a vacuum pipeline from a light source incident to an exit direction. As shown in FIG. 1, the experimental light source is incident from the right side of the second-level differential pumping assembly E and reaches the in-situ experimental device located in the experimental station through the vacuum pipeline, and all modules are mutually matched to realize the in-situ experimental function and effectively protect the front end light beam line.
The gold mesh unthreaded hole component C comprises a reflector C-10 and an unthreaded hole plate body C-11, and the light path sequentially passes through the unthreaded hole plate body C-11 and the reflector C-10.
The reflector C-10 is provided with an oblique cut surface with a through hole in the middle, and the oblique cut surface is opposite to a window of an observation port on the experiment station A; the reflector C-10 may be 314 stainless steel in particular, and may be in the shape of a chamfered cylinder. The middle part is provided with a through hole which is a square through hole, and the size of the through hole is set to be 4mm multiplied by 5mm according to the size calculation of the light path at the position. The included angle between the oblique cutting plane and the ground is 45 degrees, the direction is opposite to the upper window, and the surface of the oblique cutting plane is a mirror polished surface and is plated with a gold film.
The middle part of the unthreaded hole plate body C-11 is provided with an unthreaded hole, and the diameter of the unthreaded hole is 2mm-6 mm. The material is 314 stainless steel and is in the shape of a perforated disc. The diameter of the light hole may be 3 mm. The vacuum cavity component A-2 has the function of slowing down the time for gas to enter a vacuum pipeline when the air pressure of the inner cavity of the vacuum cavity shell in the vacuum cavity component A-2 is increased. The structure can be replaced by holes with other diameters or ultrathin silicon nitride windows and the like arranged at the unthreaded holes according to the requirements; the through hole and the unthreaded hole form a double-unthreaded hole structure, and the double-unthreaded hole structure is used for prolonging the time of gas passing through a pipeline and protecting the safety of a beam line optical device.
It can be known from the above description that, in the vacuum system for in-situ soft X-ray absorption spectroscopy experiments provided in the embodiment of the present application, the diameter of the optical aperture is 2mm to 6mm, the diameter of the optical aperture is reduced, conductance is reduced, and the reflector C-10 adopts the reflector through hole and the optical aperture to form a dual-optical-aperture structure, so as to prolong the time for the gas and liquid samples to enter the beam line vacuum pipeline, provide enough time for the valve to respond, and then close the valve in time, thereby reducing damage to the front-end optical device. Specifically, it was calculated that when the vacuum level in the vacuum chamber housing of station a varied beyond a set value, the time required for the gas to pass through a 2.2m beam line to affect the optics was greater than 100 ms.
The experiment station A comprises an XY moving platform A-1 for installing an in-situ experiment device and a vacuum cavity component A-2:
the XY moving platform A-1 is used for installing an in-situ device, and the XY moving platform A-1 can be a compact moving platform; the mounting port of the XY moving platform A-1 can be adjusted along the direction vertical to the ground and parallel to the ground, and the mounting port of the XY moving platform A-1 is over against the X-ray light source. The XY moving platform A-1 is used for installing an in-situ experiment device, the XY moving platform A-1 can be precisely adjusted in two directions perpendicular to the X-ray, the directions are perpendicular to the ground and parallel to the ground respectively, the adjusting range is +/-12.5 mm, and the adjusting precision is higher than 10 mu m.
Specifically, the vacuum cavity assembly A-2 comprises a fast valve sensor A-2-10 and a vacuum cavity shell connected with the XY moving platform A-1, the cavity of the vacuum cavity shell can be hemispherical, specifically, the vacuum cavity shell can be of a hemispherical cavity structure, and the mode that the platform surface is directly contacted with a large flange on the back surface of the vacuum cavity can be replaced. The vacuum chamber housing may also be of a semi-cylindrical or other small design with the aim of minimizing the pumping chamber volume. The vacuum cavity shell is used for installing a detector and other equipment related to the in-situ experimental device. Specifically, the XY moving stage a-1 was flange-fixed to the vacuum chamber housing by CF 63.
When the hollow cavity shell can be in a hemispherical cavity shell structure, the diameter of a hemisphere of the hemispherical cavity shell is 300mm, the wall thickness is 3mm, and the material is 316 stainless steel. The rear plane of the cavity body shell is sealed through a knife edge flange, and the flange surface is connected with a CF63 knife edge flange and an XY moving platform A-1 through a vacuum pipeline with the diameter of 60 mm.
The front hemispherical surface of the vacuum cavity shell is provided with nine connecting ports which are distributed as shown in figure 3, namely a first observation port A-2-1, a second observation port A-2-2, a third observation port A-2-3, a detector mounting port A-2-4, an X-ray source inlet A-2-5, a detector mounting port A-2-6, a spare air pumping system mounting port A-2-7, a spare detector mounting port A-2-8 and a fast valve sensor mounting port A-2-9. (Note: a plane parallel to the ground is defined as a horizontal plane and a plane perpendicular to the ground is defined as a vertical plane.
The first observation port A-2-1, the second observation port A-2-2 and the third observation port A-2-3 are CF35 flange ports, and are provided with CF35 windows for accurate positioning of an in-situ device before an in-situ experiment is carried out. The included angles of the first observation port A-2-1, the horizontal plane and the vertical plane are both 45 degrees, and the first observation port A-2-1 is used for observing the relative positions of the in-situ device and the detector arranged at the detector installation port A-2-6. The second observation port A-2-2 is positioned in the direction symmetrical to the first observation port A-2-1, and has an included angle of 45 degrees with the horizontal plane and the vertical plane, and is used for observing the relative positions of the in-situ device and the detector arranged at the detector mounting port A-2-4, and the third observation port A-2-3 has an included angle of 30 degrees with the horizontal plane and is used for observing the relative positions of the in-situ device and the X-ray light incident from the X-ray source inlet A-2-5. The observation port can be additionally provided with a camera for visual control.
The specification of the detector mounting port A-2-4 is a CF35 flange port, and the included angle between the detector mounting port A-2-4 and a vertical plane is 30 degrees. The purpose of which is to mount a photodiode of one of the detectors.
The specification of an X-ray source inlet A-2-5 is a CF63 flange port, the included angles between the flange port and a vertical plane and the included angles between the flange port and a horizontal plane are both 0 degree, and the X-ray source inlet A-2-5 is connected with a first-stage differential pumping assembly B through a CF63 welding corrugated pipe. It acts as an X-ray inlet, coaxial with the flange opening of the back XY moving stage a-1.
The detector mounting port A-2-6 and the detector mounting port A-2-4 are in symmetrical positions, are CF35 flange ports in specification, and form an included angle of 30 degrees with a vertical plane. A photomultiplier detector for mounting the second detector. The positions of the two detectors can be interchanged between the detector mounting port A-2-4 and the detector mounting port A-2-6.
And a spare air exhaust system mounting port A-2-7. The standard is CF63 flange mouth, and the included angle between the CF63 flange mouth and the vertical plane and the horizontal plane is 50 degrees. The function of the vacuum chamber is to install a standby air pumping system for recovering the vacuum of the vacuum chamber.
The spare detector mounting port A-2-8 is a CF35 flange port, and has an included angle of 30 degrees with the horizontal plane. Can be used for the installation of additional detectors such as silicon drift detectors and the like. When not installed, a CF35 blind plate can be additionally arranged at the flange opening.
The specification of the quick valve sensor mounting port A-2-9 is a CF35 flange port, and the included angles between the quick valve sensor mounting port A and the horizontal plane and the vertical plane are both 45 degrees. It acts as an interlock sensor for the quick valve at the front end of the installation system.
This application can be for hemisphere cavity body housing structure with the vacuum cavity body shell, when guaranteeing that each structure can install, avoids the installation mutual interference, reduces the volume of cavity in the vacuum cavity body shell. Namely, the vacuum cavity design is adopted, and the diameter is reduced as much as possible, so that the volume of the inner cavity can be greatly reduced, and the air extraction time is shortened. The vacuum cavity is connected with a light beam line by a CF63 standard flange, the cavity material is special ultra-high vacuum 304 stainless steel and is designed with flange openings for connecting all parts, the vacuum degree of the cavity in the background cavity shell is higher than 2 multiplied by 10-8mbar。
The vacuum cavity shell is used for installing a detector, a third turbo molecular pump A-2-13 and a flange port of a window, and the included angle between the horizontal plane and the vertical plane is 30 degrees, 45 degrees or 50 degrees. The angle can be replaced by other angles through calculation according to different installation devices.
The quick valve sensor A-2-10 is arranged on the vacuum cavity shell, and the quick valve sensor A-2-10 detects the vacuum degree in the vacuum cavity shell; the fast valve sensor A-2-10 and the vacuum fast valve E-1 of the second-stage differential pumping assembly E form an interlocking system, and when the air pressure in the vacuum cavity shell is higher than a set value, a signal is transmitted to the vacuum fast valve E-1 to close the vacuum fast valve E-1, so that the optical element is protected from being influenced.
The first stage differential pumping assembly B is typically used to obtain and maintain a vacuum in the strand vacuum chamber. The gold mesh aperture component C is a key component of the system, and mainly has the functions of measuring photocurrent in real time and reducing the influence of sudden rise of air pressure in the vacuum cavity on a front-end optical element during experiments.
The secondary differential pumping assembly E comprises a vacuum fast valve E-1 for closing and communicating a vacuum pipeline between a vacuum cavity where an optical device at the front end of the secondary differential pumping assembly E is located and the secondary differential pumping assembly E, the vacuum fast valve E-1 is connected with a fast valve sensor A-2-10 and is connected with the vacuum fast valve E-1 of the secondary differential pumping assembly E, and when the experiment station A runs normally, the vacuum fast valve E-1 is in an open state, so that X rays can be incident to the experiment station. When the fast valve sensor A-2-10 detects that the air pressure in the vacuum cavity is higher than a set value or is manually closed, the vacuum fast valve E-1 is closed within 40ms to protect the front-end optical element. . The flange specification of the vacuum fast valve E-1 is CF35 knife edge flange, which is used for closing and communicating the vacuum cavity where the front end optical device is located and the second-stage differential pumping assembly E. By adopting the design of the quick valve, after the quick valve sensor A-2-10 in the vacuum cavity responds, the vacuum quick valve E-1 can be closed within 40ms, so that the optical device is protected from being influenced. 1 set of quick valves is adopted to protect optics, the valves are closed when the air pressure exceeds a set value, and the response time is not more than 100 ms.
The length from the center of the vacuum cavity to the vacuum fast valve E-1 of the experimental system is 2.2m, and the length of the experimental system can be adjusted according to different wire harnesses installed in the experimental system. One common method is to adjust the length of the tube between the gold mesh aperture assembly C and the diaphragm assembly D.
In one embodiment, the laboratory station A further comprises a first vacuum gauge A-2-11 mounted on the vacuum chamber housing, the first vacuum gauge A-2-11 being adapted to read the vacuum level in the chamber of the vacuum chamber housing, wherein the conventional read vacuum level is read via a display screen on a controller of the first vacuum gauge A-2-11; the first vacuum gauge pipe A-2-11 is arranged at a mounting port A-2-7 of a standby air exhaust system. The vacuum protection device is used for reading the vacuum degree in the vacuum cavity and is interlocked with the first pneumatic gate valve B-2 to form a vacuum protection system.
The first-stage differential pumping assembly B comprises a first three-way connecting pipeline B-1, a first pneumatic gate valve B-2, a second pneumatic gate valve B-3, a first turbo molecular pump B-4 and a pipeline support B-5.
A first interface of the first three-way connecting pipeline B-1 is connected with the vacuum cavity shell; the flange specification of the first three-way connecting pipeline B-1 is a CF63 knife edge flange, and the material is 304 stainless steel. Which functions to provide a vacuum connection. Three connectors are respectively connected with a vacuum cavity shell A-2, a first pneumatic gate valve B-2 and a second pneumatic gate valve B-3. And the bottom of the interface is welded with a square fixing plate which is connected with a pipeline bracket B-5 through a bolt.
Specifically, the first pneumatic gate valve B-2 is used for closing and communicating a pipeline between the first-level differential pumping assembly B and the gold mesh unthreaded hole assembly C, the first pneumatic gate valve B-2 and the first vacuum gauge pipe A-2-11 form a vacuum interlocking system, and the first pneumatic gate valve B-2 is connected with a second interface of the first tee joint connecting pipeline B-1. When the experiment station operates, the first pneumatic gate valve B-2 is in an open state, so that X rays can be incident to the experiment station. When the first vacuum gauge pipe A-2-11 monitors that the air pressure in the vacuum cavity shell is higher than a set value or is manually closed, the first pneumatic gate valve B-2 is in a closed state and is used for protecting the front-end optical element. The porosity of the gold mesh is not less than 80%, and the gold mesh can be designed to have higher or lower light passing rate according to different light intensities.
And the second pneumatic gate valve B-3 is connected with a third interface of the first three-way connecting pipeline B-1. The second pneumatic gate valve B-3 and the first vacuum gauge A-2-11 form a vacuum interlocking system, and the second pneumatic gate valve B-3 is normally in an open state. When the pressure in the vacuum cavity is higher than the set value or is manually closed, the vacuum cavity is in a closed state and is used for protecting the first turbo-molecular pump B-4B-4.
The second pneumatic gate valve B-3 is used for closing and communicating a pipeline between the first tee joint connecting pipeline B-1 and the first turbo molecular pump B-4; the flange specification of the first turbo molecular pump B-4 is CF63 knife-edge flange, and one end of the first turbo molecular pump B-4 is connected with the second pneumatic gate valve B-3 to be used as a main pump for maintaining and obtaining vacuum of the vacuum cavity under the conventional condition. The first turbomolecular pump B-4 is normally operating at full speed and will be shut down when system maintenance is required.
The material of the pipeline bracket B-5 is No. 45 steel, the middle part of the vertical square rod is hollow, the thickness of steel is 8mm, and the thickness of steel of the top and bottom horizontal support plates is 10 mm. The vertical rod and the support plate are welded to form an integral support. The top and the bottom of the pipeline bracket B-5 are respectively connected with the first three-way connecting pipeline B-1 and the ground through bolts.
The secondary differential pumping assembly E is used for obtaining and maintaining branch line vacuum under normal conditions, plays an important role in protecting front-end optical devices, and further comprises a second three-way connecting pipeline E-2, a third pneumatic gate valve E-3, a second turbo molecular pump E-4 and a pipeline support E-5.
A first interface of the second three-way connecting pipeline E-2 is connected with the diaphragm assembly D, and a second interface of the second three-way connecting pipeline E-2 is connected with the vacuum fast valve E-1. The flange specification is CF63 knife edge flange, and the material is 304 stainless steel. Which functions to provide a vacuum connection. And three connecting ports of the pneumatic diaphragm valve are respectively connected with the diaphragm assembly D, the vacuum fast valve E-1E-1 and the third pneumatic gate valve E-3. The bottom of the second three-way connecting pipeline E-2 is welded with a square fixing plate and is connected with a pipeline bracket E-5 through a bolt. The two ends of the three-way connecting pipeline are also connected with adapter pieces from CF63 to CF35, and the adapter pieces are used for matching the sizes of the vacuum fast valve E-1 and the pipeline flange.
The third port of the second tee joint pipeline E-2 is connected with a third pneumatic gate valve E-3, the third pneumatic gate valve E-3 and the first vacuum gauge pipe A-2-11 form a vacuum interlocking system, and the third pneumatic gate valve E-3 is in an open state under normal conditions. When the air pressure in the vacuum cavity of the vacuum cavity assembly A-2 is higher than a set value or is manually closed, the vacuum cavity is in a closed state and is used for protecting the second turbo molecular pump E-4.
And the third pneumatic gate valve E-3 is used for closing and communicating the second three-way connecting pipeline E-2 and the second turbo molecular pump E-4. The flange specification of the second turbo molecular pump E-4 is CF63 knife edge flange, and the second turbo molecular pump E-4 and the third pneumatic gate valve E-3 are connected as a main pump for obtaining and maintaining diaphragm vacuum degree under the conventional condition. The second turbomolecular pump E-4 is normally operating at full speed and will be shut down when system maintenance is required.
The material of pipeline bracket E-5 is 45 # steel, the middle part of vertical square rod is hollow, the thickness of steel is 8mm, and the thickness of top and bottom horizontal support plate steel is 10 mm. The vertical rod and the support plate are welded to form an integral support. The top and the bottom of the bracket are respectively connected with a second three-way connecting pipeline E-2 and the ground through bolts.
In a specific embodiment, the inner diameters of the air exhaust pipeline of the first-stage differential pumping assembly B and the air exhaust pipeline of the second-stage differential pumping assembly E are both 45mm to 55mm, and specifically, the inner diameters of the air exhaust pipeline of the first-stage differential pumping assembly B and the air exhaust pipeline of the second-stage differential pumping assembly E are 50 mm.
The experiment station A further comprises a fourth pneumatic gate valve A-2-12, a third turbo molecular pump A-2-13, a cavity support A-3, a six-axis adjusting device A-4 and a base A-5.
When the inner cavity of the vacuum cavity shell needs to be vacuumized by an auxiliary pump, the vacuum cavity shell is opened, so that the air pumping process is accelerated; a-2-12: CF63 pneumatic gate valve. Used for separating or communicating the A-2-13 molecular pump and the vacuum cavity. The gate valve is closed under the normal condition, and the vacuum cavity is opened to accelerate the air exhaust process when the auxiliary pump is needed to vacuumize.
And the fourth pneumatic gate valve A-2-12 is used for separating or communicating the third turbomolecular pump A-2-13 and the inner cavity of the vacuum cavity shell. -2-13: a turbomolecular pump. The specification of the flange is CF63 knife edge flange, and one end of the molecular pump is connected with A-2-12 to be used as an auxiliary pump for assisting in realizing the quick acquisition of vacuum of the vacuum cavity. The molecular pump is normally in an off state and will be turned on when a vacuum needs to be rapidly obtained.
The cavity support A-3 is used for supporting a vacuum cavity shell, and the material of the cavity support A-3 is 304 stainless steel. The cavity support A-3 is formed by welding a bottom plate, a triangular support plate and a vertical support frame. The vacuum cavity shell is connected with the cavity support A-3 through a screw rod. The triangular supporting plates are uniformly distributed and used for improving the stability of the cavity. The welding position between the vertical support frame and the triangular support plate is obtained through simulation, so that the gravity center of the cavity body can be positioned on the same plane of the vertical support frame. The cavity support A-3 has the functions of supporting and adjusting the position of the vacuum cavity, and is fixed on the ground through a screw, and the ground penetration depth of the screw is not less than 150mm so as to improve the stability of the system.
The six-axis adjusting device A-4 is used for adjusting the axial displacement and the rotation angle of the vacuum cavity shell; as shown in FIG. 2, the six-axis adjustment mechanism A-4 consists of six independently adjustable movable rods. The six-axis adjusting device A-4 comprises six independently adjustable moving rods, each moving rod comprises a pipe body with internal threads in the middle section and joint nuts positioned at two ends of the pipe body, and two ends of each moving rod are respectively connected with the cavity support A-3 and the base A-5 through screws; the six moving rods are respectively two first moving rods for adjusting the horizontal position of the vacuum cavity shell and four second moving rods for adjusting the height and the rotating angle of the vacuum cavity shell.
The moving rod is made of chrome-plated 45 # steel, the middle section of the moving rod is a steel pipe with internal threads, and the moving rod is made of 45 # steel with the surface subjected to anodic oxidation. Two ends of each movable rod are respectively connected with the cavity support A-3 and the base A-5 through screws. Two transverse first moving rods are used for adjusting the horizontal angle of the cavity support A-3. And the four second moving rods which are obliquely fixed in the vertical planes are used for adjusting the height of the cavity support A-3 and the relative position of the cavity support A-3 and incident X-rays. The six-axis adjusting device A-4 can realize free adjustment of the vacuum cavity assembly A-2 in six dimensions (three axial displacements and three rotation angles in three-dimensional space). The system adopts a position adjusting system with six moving rods matched in two places, and a hexagonal moving platform (Hexapod) or a moving platform formed by matching mutually vertical screw rods and a track plate can also be adopted according to requirements. The function of the device is to perform three-axis adjustment and three-axis rotation adjustment.
The six-axis adjusting device A-4 is arranged on the base A-5. Specifically, the base A-5 is preferably a granite base. The base A-5 is made of a combination of granite powder and a polymer. The upper part and the bottom of the base A-5 are provided with threaded holes for fixing the six-axis adjusting device A-4 on the base A-5 and fixing the base A-5 on the ground. The design of the base A-5 preferably lowers the center of gravity of the experiment station and improves the stability. In addition, the base made of the material can reduce the influence of ground vibration on the experiment station. The base A-5 can also be replaced by a supporting base made of marble, pure granite or steel or aluminum profiles according to requirements.
The gold mesh unthreaded hole assembly C further comprises a gold mesh fixed rod C-1, a gold mesh current reading port C-2, a welding corrugated pipe C-3, a first six-way pipeline C-4, a third three-way connecting pipeline C-5, a hollow manual valve C-6, a moving rod C-7, a gold evaporation source C-8 and a support frame C-9.
The gold mesh fixing rod C-1 is a rotating shaft fixed in the center of the flange, the gold mesh is fixed at the front end of the rotating shaft, and the gold mesh is positioned on an X-ray light path in a working state; the flange of the gold mesh fixing rod C-1 is a CF35 knife edge flange, and the structure of the flange is a rotating shaft fixed in the center of the flange. The gold net is fixed at the front end of the rotating shaft and is positioned on an X-ray light path in a working state.
The gold mesh current reading port C-2 is an electrode fixed in the center of the flange, and the electrode is connected with a gold mesh at the front end of the gold mesh fixing rod C-1 and insulated from an external pipeline; the flange of the gold mesh current reading port C-2 is a CF16 knife edge flange, and the structure is an electrode fixed in the center of the flange, and the electrode is connected with a gold mesh at the front end of a gold mesh fixing rod C-1 and insulated from an external pipeline. When the X-ray irradiates on the gold net, photocurrent is generated and collected by the electrode on the gold net current reading port C-2, and the photocurrent is used for calibrating the luminous flux of the X-ray in real time.
The welding corrugated pipe C-3 is used for connecting an external pipeline of the gold mesh unthreaded hole assembly C and the diaphragm assembly D; the specification of a flange of the welding corrugated pipe C-3 is a CF35 knife edge flange which is used for connecting a gold mesh aperture component C and a diaphragm component D. Because the gold mesh unthreaded hole component C needs to be optically collimated to realize the function, the position of the gold mesh unthreaded hole component C needs to be adjusted by a six-axis adjusting device A-4. The stress generated by this process can be reduced by the bellows. The length of the welded bellows C-3 can be adjusted as desired.
The flange specification of the first six-way pipeline C-4 is CF35 knife edge flange, and the first six-way pipeline C-4 has six connecting ports. Along the light path direction, the front end interface of the first six-way pipeline C-4 is connected with the welding corrugated pipe C-3 and is used for being communicated to the diaphragm assembly D, and the upper end interface of the first six-way pipeline C-4 is provided with a first window which is used for observing the content of the gold in the gold evaporation source C-8. And a second window is arranged at the left end interface of the first six-way pipeline C-4 and is used for observing the position and the angle of the gold mesh. The right end interface of the first six-way pipeline C-4 is connected with a gold mesh fixing rod C-1. The lower end interface of the first six-way pipeline C-4 is connected with a gold evaporation source C-8.
The rear end interface of the first six-way pipeline C-4 is connected with the first interface of the third three-way connecting pipeline C-5 to communicate the gold mesh with the pipeline where the unthreaded hole is located, so that a closed space required for maintaining the pipeline is formed.
The flange specification of the third three-way connecting pipeline C-5 is CF35 knife edge flange, and the third three-way connecting pipeline C-5 has three connecting ports in total. The front end along the light path direction is connected with the six-way pipeline to form a closed space required by the maintenance pipeline. The rear end is connected with a hollow manual valve C-6, and the upper end of a third three-way connecting pipeline C-5 forms a second interface for installing a CF35 window. The bottom of the three-way pipeline is welded with a half-moon-shaped fixing plate which is used for being connected with an upper plate of the support frame C-9 through a screw rod. The center of the pipeline is provided with a reflector C-10.
The middle part of the hollow manual valve C-6 is provided with a through hole for installing a unthreaded hole plate body C-11, and the upper part of the hollow manual valve C-6 is provided with a handle which can arrange the unthreaded hole of the unthreaded hole plate in the center of a light path or move out through rotation; the hollow manual valve C-6 is a CF35 hollow manual valve. The middle part of the hollow manual valve C-6 is provided with a through hole which is used for installing a unthreaded hole plate body C-11. The light hole can be arranged at the center of the light path or moved out through the handle at the upper part of the valve through rotation.
Wherein, the moving rod C-7 can be a telescopic rod with adjustable length. The material of the moving rod C-7 is 45 # steel with the surface being anodized. The rod main body of the moving rod C-7 is a hollow steel pipe with threads, the upper end and the lower end of the moving rod C-7 are connected with joint nuts and are fixed on an upper plate of the support frame C-9 and a mounting plate of a welding corrugated pipe C-3, and a first six-way pipeline C-4 and a third three-way connecting pipeline C-5 are mounted on the gold mesh unthreaded hole assembly through screws. The number of the moving rods C-7 is 6, three of the moving rods are horizontally arranged, and the other three moving rods are vertically arranged. The middle part of the movable rod C-7 is rotated to adjust the relative position of the threaded connection between the hollow steel pipe and the screw, so that the use length of the movable rod C-7 is changed, and the positions of the gold mesh and the unthreaded hole are adjusted.
The gold evaporation source C-8 is a crucible connected with double electrodes, and gold particles are placed in the middle of the crucible and used for carrying out in-situ gold film plating on a gold mesh; the structure is a ceramic crucible connected by double electrodes, and gold particles are placed in the middle of the crucible. The gold particles can be melted by electrifying the electrodes, so that the gold net is plated with the gold film in situ.
The light intensity is measured by adopting a gold net, and the background current of a measuring circuit is not more than 0.1 pA. The light transmittance of the gold net is not less than 80%, and the gold net can be completely moved out of the light path and is provided with an in-situ gold evaporation source C-8.
The vacuum interlocking and program control movement adopts LabVIEW software, can read the vacuum degree in real time and carry out on-off control on the pneumatic gate valve, the quick valve and the corresponding molecular pump. The program has openness, and can be programmed to carry out function expansion so as to meet the requirement of system upgrading later.
The support frame C-9 comprises an upper plate and a lower plate, the upper plate is used for installing a pipeline of the gold mesh unthreaded hole assembly C, the lower plate is connected with the ground, the moving rod C-7 is used for adjusting the height and the horizontal rotation angle of the upper plate, and specifically, the moving rod C-7 is a rod body structure with the telescopic length. The support frame C-9 is connected by a moving rod C-7. The upper plate is connected with a pipeline where the metal net and the unthreaded hole plate body C-11 are located, and the lower square rigid frame is connected with the ground through a screw rod or can be directly poured through concrete. The material of the support frame C-9 is No. 45 steel, and can be changed into other types of materials such as aluminum profiles, 304 stainless steel, 316 stainless steel and the like;
the square steel adopted by the support frame C-9 is of a hollow structure, the wall thickness of the square steel is 8mm, other thicknesses can be replaced, concrete can be poured into the inner space, and the like.
The diaphragm assembly D comprises an adjustable square diaphragm D-1, an electric control linear driver D-2, a manual linear driver D-3, a second six-way pipeline D-4 and a second vacuum gauge pipe D-5.
The number of the adjustable square apertures D-1 is two, and the two adjustable square apertures are respectively horizontally installed and vertically installed; the adjustable square aperture D-1 is used for adjusting the size of light passing through and mainly comprises a telescopic rod D-1-1 and aperture accessories, and the structure of the adjustable square aperture D-1 is described as follows:
the adjustable square aperture D-1 comprises a telescopic rod D-1-1, an aperture upper layer adjusting plate D-1-2, a diaphragm fixing flange D-1-3, an aperture lower layer adjusting plate D-1-4 and a step slide block D-1-5.
The specification of the flange of the telescopic rod D-1-1 is a CF16 knife edge flange. The flange is connected with a rotary telescopic rod D-1-1, and the center of the rod can be screwed in and out through threads to be telescopic by rotating a rotating shaft at the upper end, namely, as shown in figure 8, the rotating shaft rotates to drive the telescopic rod D-1-1 to ascend or descend. The front end of the telescopic rod D-1-1 is fixedly connected with the aperture upper layer adjusting plate D-1-2, and particularly can be connected through a screw rod.
The upper adjusting plate D-1-2 of the light ring is a rectangular stainless steel plate with a middle hole, and the material is 304 stainless steel. The upper end of the upper adjusting plate D-1-2 of the light ring is provided with a circular through hole which is connected with the telescopic rod D-1-1 through two screw rods. The middle hole is connected with a step slide block D-1-5 and is used for adjusting the size and the parallelism of the aperture. The size is adjusted by screwing in and out the thread of the telescopic rod D-1-1. Parallelism is measured and adjusted at assembly by the assembly tool.
The diaphragm fixing flange D-1-3 is a double-layer double-sided flange, one side of the upper end flange is a CF16 knife edge, and the other side of the upper end flange is a CF35 knife edge. The end face of CF16 is connected with the telescopic rod D-1-1, and the end face of CF35 is connected with the lower double-sided flange. Both ends of the lower double-sided flange are CF35 knife edges. The center of the lower end of the diaphragm is provided with a threaded hole which is connected with an aperture lower layer adjusting plate D-1-4 through a screw rod.
The structure of the aperture lower layer adjusting plate D-1-4 is a U-shaped rectangular plate with an arc square hole, and the material is 304 stainless steel. The upper end of the diaphragm lower adjusting plate D-1-4 is fixedly connected with the diaphragm fixing flange D-1-3 through a screw rod, and a lower arc square hole and the lower edge of the diaphragm upper adjusting plate D-1-2 form a diaphragm boundary. The relative position between the upper layer and the lower layer is adjusted through the telescopic rod D-1-1 to enlarge and reduce the aperture.
The step slide block D-1-5 is in the shape of a step cylinder with a through hole. The material is beryllium copper. The step slide block is connected with an aperture lower layer adjusting plate D-1-4 through a through hole and a screw rod, and the upper part of the step D-1-5 is in sliding contact with an aperture upper layer adjusting plate D-1-2. When the telescopic rod D-1-1 moves, the step slide block D-1-5 can keep the upper adjusting plate D-1-2 of the aperture and the lower adjusting plate D-1-4 of the aperture to slide in parallel. The size of the diaphragm in the adjustable square diaphragm D-1 is adjusted by screwing the telescopic rod D-1-1 into and out of the adjusting diaphragm lower layer adjusting plate D-1-4 and the step sliding block D-1-5 in relative positions.
The electric control linear driver D-2 adjusts the position of the diaphragm in the vertical direction, the electric control linear driver D-2 is structurally a single-shaft moving platform with two CF35 knife edge flanges connected through a corrugated pipe, and the platform is driven by a motor and can adjust the distance between the flanges. The upper flange is connected with an adjustable square aperture D-1, and the lower end is connected with a second six-way pipeline D-4. The electric control linear driver D-2 can continuously drive the adjustable square aperture D-1 to move in the vertical direction and is used for adjusting the position of the adjustable square aperture D-1 in the vertical direction.
The manual linear driver D-3 adjusts the relative position of the aperture and the optical path in the horizontal direction, the manual linear driver D-3 is similar to the electric control linear driver D-2, the structure of the manual linear driver D-3 is also a single-shaft moving platform with two CF35 knife-edge flanges connected through a corrugated pipe, and the difference is that the platform is manually adjusted in position through a handle. The component is arranged at the horizontal position of a second six-way pipeline D-4 and is used for adjusting the relative position of the adjustable square aperture D-1 and the light path in the horizontal direction and reducing stray light entering an experimental station. The position of the adjustable square aperture D-1 relative to the light path is adjusted through the electric control linear driver D-2 and the manual linear driver D-3.
The two second six-way pipelines D-4 are connected to form a vacuum pipeline, the upper end interface of the first second six-way pipeline D-4 along the light path direction is connected with the electric control linear driver D-2, and the front end interface of the first second six-way pipeline D-4 is provided with a corrugated pipe and is connected with the secondary differential pumping component E through a pipeline with adjustable length; the upper end interface of the second six-way pipeline D-4 is connected with a window, the left end interface of the second six-way pipeline D-4 is connected with a manual linear driver D-3, and blind plates are detachably mounted on other interfaces of the second six-way pipeline D-4 for standby use. The flange specification of the second six-way pipeline D-4 is a CF35 knife edge flange, and the material is 304 stainless steel. The second six-way pipeline D-4 is connected with the bottom support frame D-6 through a support plate.
The diaphragm assembly D moves by a distance not less than 20mm in the direction perpendicular to the optical axis, and the linear driver is moved by program control. The size interval of the diaphragm switch is not less than 0-10 mm. The unthreaded hole plate body C-11 and an observation device thereof are fixed on a six-axis supporting and adjusting platform formed by a movable rod C-7 and a supporting frame C-9, and the moving distance of the unthreaded hole plate body C-11 in each direction is not less than 3 mm.
And a second vacuum gauge D-5 is used for measuring the vacuum degree of the inner cavity of the diaphragm assembly D, and a right end interface of the first and second six-way pipelines D-4 is connected with the second vacuum gauge D-5. The function is to measure the vacuum at the diaphragm. The flange specification is CF35 knife edge flange, adopts cold cathode rule to reduce the influence of stray light.
The bottom support frame D-6 is made of 45 # steel with the surface anodized and is formed into a main body shape through welding. The upper end of the bottom support frame D-6 is connected with the second six-way pipeline D-4 through a clamping ring and a screw rod to provide support, and the lower part of the bottom support frame D-6 is fixed on the ground through the screw rod.
The inner diameter of the pumping ports of the first turbo molecular pump B-4, the second turbo molecular pump E-4 and the third turbo molecular pump A-2-13 is 55mm-65 mm.
In addition to a pump which needs to maintain vacuum normally, a third turbo molecular pump A-2-13 which is specially used for recovering vacuum is additionally arranged on the side face of a vacuum cavity of the vacuum cavity component A-2. When the vacuum needs to be recovered, the fourth pneumatic gate valve A-2-12 at the front end of the third turbo molecular pump A-2-13 can be opened, and the time for obtaining the high vacuum is shortened by increasing the total pumping speed.
In addition, this application adopts the mode that increases the pipeline internal diameter of bleeding, vacuum cavity inner wall passivation to further reduce the time of bleeding. The mode that a two-stage differential pump is matched with the special design of the diameter of a pipeline is adopted, a large-caliber pipeline (60mm inner diameter) is adopted at the air exhaust position to improve the flow conductance, so that the air exhaust efficiency is improved, and the small-caliber pipeline is adopted at other parts to reduce the flow conductance and prolong the time for gas to pass through.
The experiment station adopts a method of separating dimension adjustment from reaction tank installation, and after the cavity position is adjusted through the six-axis platform of the experiment station, the focusing point of light can be ensured at the sample point of the reaction device only by directly installing the reaction device, so that the adjustment time is greatly shortened, and the experiment efficiency is improved. As above, the reaction apparatus is used for sample support in performing in situ X-ray absorption spectroscopy experiments. The mounting is performed at the mounting port of the XY moving stage A-1.
In the traditional in-situ reaction, because the reaction device needs to be adjusted horizontally, vertically and angularly, the sample point of the reaction device is positioned by translation of three dimensions of XYZ and rotation around the Z axis. This patent structure reduces four removals into two to accurate fixed reaction unit length makes the reaction cell install back sample point promptly and is located the focus of light through the design, and two directions XY also need not to adjust under the normal condition, have consequently shortened the regulation time.
This application adopts 3 sets of turbine molecular pump air pumping systems, corresponds pneumatic slide valve and need can connect into the true light beam line of lightThe air interlocking system is controlled by a program, and can be automatically closed when the air pressure exceeds a set value, and the default set value is 5 multiplied by 10-7mbar。
The first vacuum gauge A-2-11 and the second vacuum gauge D-5 adopt cold cathode type vacuum gauges, and the limit value of vacuum measurement is not lower than 1 multiplied by 10-10mbar. The vacuum level can be programmed and connected to a vacuum interlock system.
The material of the pipes and the chamber body of the vacuum system is 304 stainless steel, and can be replaced by 316 stainless steel, aluminum or other materials which can meet the requirements of an ultrahigh vacuum system according to needs.
The flange of the system can be a CF63, CF35 or CF16 edge flange according to requirements, and can be replaced by other types of flanges such as a quick-release (KF) flange.
The CF63 knife flange is adopted by each molecular pump, and larger molecular pumps such as CF100 or CF150 based large molecular pumps can be adopted if the pumping speed needs to be adjusted.
The vacuum line is located at a distance of about 1.3m from the ground and may vary in height depending on the installation of the wire harness.
The software used for the vacuum chain is LabView, and can be replaced by other types of software according to needs.
In the design, the experiment station base A-5, the pipeline support B-5, the support frame C-9, the bottom support frame D-6 and the pipeline support E-5 are preferably designed symmetrically, the shapes of the experiment station base A-5, the pipeline support B-5, the support frame C-9, the bottom support frame D-6 and the pipeline support E-5 are optimized in a calculation mode according to the characteristics of an installation system, and when other sizes or more functional components are additionally installed, the heights and the shapes of the base and the support frame C-9 can be correspondingly changed so as to optimize the stability of the system.
In the application, the adjusting range of the aperture is preferably 0-10mm, and the adjusting range of the aperture in the diaphragm can be correspondingly changed according to different beam lines.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A vacuum system for in-situ soft X-ray absorption spectroscopy experiments is characterized by comprising a secondary differential pumping assembly (E), a diaphragm assembly (D), a gold mesh aperture assembly (C), a primary differential pumping assembly (B) and an experiment station (A) which are sequentially connected from a light source to an emergent direction through a vacuum pipeline;
the gold mesh aperture assembly (C) comprises:
the reflecting mirror (C-10) is provided with an oblique cutting surface with a through hole in the middle, and the oblique cutting surface is opposite to a window of an observation port on the experiment station (A);
and the unthreaded hole plate body (C-11), the unthreaded hole is arranged in the middle of the unthreaded hole plate body (C-11), and the diameter of the unthreaded hole is 2mm-6 mm.
2. Vacuum system usable for in situ soft X-ray absorption spectroscopy experiments according to claim 1 characterized in that said experimental station (a) comprises:
the X-Y moving platform (A-1) is used for mounting an in-situ experimental device, the mounting port of the X-Y moving platform (A-1) can be adjusted along the direction vertical to the ground and parallel to the ground, and the mounting port of the X-Y moving platform (A-1) is over against the X-ray light source;
a vacuum chamber assembly (a-2) for mounting a probe and apparatus associated with an in situ experimental setup thereof, said vacuum chamber assembly (a-2) comprising:
a vacuum chamber housing connected to the XY moving platform (A-1);
a fast valve sensor (A-2-10) mounted on the vacuum cavity housing, the fast valve sensor (A-2-10) detecting the vacuum degree in the cavity of the vacuum cavity housing;
the secondary differential pumping assembly (E) comprises a vacuum fast valve (E-1) which is used for closing and communicating a vacuum pipeline between a vacuum cavity where an optical device at the front end of the secondary differential pumping assembly (E) is located and the secondary differential pumping assembly (E), the vacuum fast valve (E-1) is connected with the fast valve sensor (A-2-10), and when the experiment station (A) normally runs, the vacuum fast valve (E-1) is in an open state, so that X rays are incident to the experiment station (A); when the fast valve sensor (A-2-10) detects that the air pressure in the vacuum cavity is higher than a set value or is manually closed, the vacuum fast valve (E-1) is closed within 40 ms.
3. The vacuum system usable for in situ soft X-ray absorption spectroscopy experiments according to claim 2, wherein said experimental station (a) further comprises a first vacuum gauge (a-2-11) mounted on said vacuum chamber housing, said first vacuum gauge (a-2-11) being used for reading the vacuum level in the vacuum chamber housing cavity;
the first-stage differential pumping assembly (B) comprises:
the first port of the first three-way connecting pipeline (B-1) is connected with the vacuum cavity shell;
the first pneumatic gate valve (B-2) is used for closing and communicating a vacuum pipeline between the primary differential pumping assembly (B) and the gold mesh unthreaded hole assembly (C), and the first pneumatic gate valve (B-2) is connected with a second interface of the first three-way connecting pipeline (B-1);
the second pneumatic gate valve (B-3), the second pneumatic gate valve (B-3) is connected with the third interface of the first tee connecting pipeline (B-1);
a first turbomolecular pump (B-4), said second pneumatic gate valve (B-3) being adapted to close and communicate the vacuum conduit between said first three-way connection conduit (B-1) and said first turbomolecular pump (B-4);
the second stage differential pumping assembly (E) further comprises:
a second three-way connecting pipeline (E-2), wherein a first interface of the second three-way connecting pipeline (E-2) is connected with the diaphragm assembly (D), and a second interface of the second three-way connecting pipeline (E-2) is connected with the vacuum fast valve (E-1);
a third pneumatic gate valve (E-3), wherein a third interface of the second three-way connecting pipeline (E-2) is connected with the third pneumatic gate valve (E-3);
a second turbo molecular pump (E-4), the third pneumatic gate valve (E-3) is used for closing and communicating the second three-way connecting pipeline (E-2) and the second turbo molecular pump (E-4).
4. The vacuum system for in-situ soft X-ray absorption spectroscopy experiments according to claim 3, wherein the inner diameters of the air pumping pipeline of the first-stage differential pumping assembly (B) and the air pumping pipeline of the second-stage differential pumping assembly (E) are both 45mm-55 mm.
5. Vacuum system usable for in situ soft X-ray absorption spectroscopy experiments according to claim 3 characterized in that said experimental station (A) further comprises:
a fourth pneumatic gate valve (A-2-12) which is opened when the cavity in the vacuum cavity shell needs to be vacuumized by an auxiliary pump, so that the air pumping process is accelerated;
the third turbo molecular pump (A-2-13) and the fourth pneumatic gate valve (A-2-12) are used for separating or communicating the third turbo molecular pump (A-2-13) and the inner cavity of the vacuum cavity shell.
6. Vacuum system usable for in situ soft X-ray absorption spectroscopy experiments according to claim 2 characterized in that said experimental station (a) further comprises:
a chamber mount (A-3) for supporting the vacuum chamber housing;
a six-axis adjustment device (A-4) for adjusting the vacuum chamber housing axial displacement and rotation angle;
a base (A-5), on which the six-axis adjustment device (A-4) is mounted.
7. The vacuum system for in-situ soft X-ray absorption spectroscopy experiments as claimed in claim 6, wherein the six-axis adjusting device (A-4) comprises six independently adjustable moving rods, each moving rod comprises a tube body with an internal thread at the middle section and joint nuts at two ends of the tube body, and two ends of each moving rod are respectively connected with the cavity support (A-3) and the base (A-5) through screws;
six the removal stick is two respectively and is used for adjusting vacuum chamber shell horizontal position's first removal stick and four second removal sticks that are used for adjusting vacuum chamber shell height and rotation angle.
8. The vacuum system usable for in situ soft X-ray absorption spectroscopy experiments according to claim 1, wherein the gold mesh aperture assembly (C) further comprises:
the gold mesh fixing rod (C-1) is a rotating shaft fixed in the center of the flange, the gold mesh is fixed at the front end of the rotating shaft, and the gold mesh is positioned on an X-ray light path in a working state;
the gold mesh current reading port (C-2) is an electrode fixed in the center of the flange, and the electrode is connected with a gold mesh at the front end of the gold mesh fixing rod (C-1) and insulated from an external pipeline;
a welding bellows (C-3) for connecting an external pipe of the gold mesh aperture assembly (C) and the diaphragm assembly (D);
the front end interface of the first six-way pipeline (C-4) is connected with the welding corrugated pipe (C-3) along the direction of the light path and is used for being communicated to the diaphragm assembly (D); the upper end interface of the first six-way pipeline (C-4) is provided with a first window; a second window is arranged at the left end interface of the first six-way pipeline (C-4); the right end interface of the first six-way pipeline (C-4) is connected with the gold mesh fixing rod (C-1);
the rear end interface of the first six-way pipeline (C-4) is connected with the first interface of the third three-way pipeline (C-5) to form a closed space required by a maintenance pipeline, the gold mesh and the pipeline where the unthreaded hole plate body (C-11) is located are communicated, and the upper end of the third three-way pipeline (C-5) forms a second interface for installing a window;
the middle part of the hollow manual valve (C-6) is provided with a through hole for installing a unthreaded hole plate body (C-11), the rear end of the third three-way connecting pipeline (C-5) is provided with a third interface along the direction of a light path to be connected with the hollow manual valve (C-6), and the upper part of the hollow manual valve (C-6) is provided with a handle which can be used for arranging the unthreaded hole of the unthreaded hole plate in the center of the light path or moving the unthreaded hole out through rotation;
a moving bar (C-7);
the gold evaporation source (C-8) is a crucible connected with double electrodes, gold particles are placed in the middle of the crucible and used for carrying out in-situ gold film plating on a gold net, and the lower end interface of the first six-way pipeline (C-4) is connected with the gold evaporation source (C-8);
the supporting frame (C-9) comprises an upper plate and a lower plate, the upper plate is used for installing a vacuum pipeline of the gold mesh unthreaded hole assembly (C), the lower plate is connected with the ground, and the moving rod (C-7) is used for adjusting the height and the horizontal rotation angle of the upper plate.
9. Vacuum system usable for in situ soft X-ray absorption spectroscopy experiments according to claim 1 characterized in that said diaphragm assembly (D) comprises:
the number of the adjustable square apertures (D-1) is two, and the two adjustable square apertures (D-1) are respectively horizontally and vertically arranged;
an electrically controlled linear drive (D-2) for adjusting the position of the adjustable square aperture (D-1) in the vertical direction;
a manual linear driver (D-3) for adjusting the relative position of the adjustable square aperture (D-1) and the optical path in the horizontal direction;
the two second six-way pipelines (D-4) are connected to form a vacuum pipeline, the upper end interface of the first second six-way pipeline (D-4) in the light path direction is connected with the electric control linear driver (D-2), and the front end interface of the first second six-way pipeline (D-4) is provided with a corrugated pipe and is connected with the secondary differential pumping assembly (E) through a pipeline with adjustable length; the upper end interface of the second six-way pipeline (D-4) is connected with a window, the left end interface of the second six-way pipeline (D-4) is connected with the manual linear driver (D-3), and other interfaces of the second six-way pipeline (D-4) are detachably provided with blind plates for standby;
and the right end interface of the first six-way pipeline (D-4) is connected with the second vacuum gauge pipe (D-5).
10. The vacuum system usable for in-situ soft X-ray absorption spectroscopy experiments according to claim 5, wherein the inner diameter of the pumping ports of the first turbo molecular pump (B-4), the second turbo molecular pump (E-4) and the third turbo molecular pump (A-2-13) is 55mm-65 mm.
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