CN113340813A - Portable ultrahigh vacuum low-temperature observation cavity with micro-area characterization function and operation method - Google Patents
Portable ultrahigh vacuum low-temperature observation cavity with micro-area characterization function and operation method Download PDFInfo
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- CN113340813A CN113340813A CN202110517081.2A CN202110517081A CN113340813A CN 113340813 A CN113340813 A CN 113340813A CN 202110517081 A CN202110517081 A CN 202110517081A CN 113340813 A CN113340813 A CN 113340813A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0332—Cuvette constructions with temperature control
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0332—Cuvette constructions with temperature control
- G01N2021/0335—Refrigeration of cells; Cold stages
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0317—High pressure cuvettes
Abstract
The invention discloses a portable ultrahigh vacuum low-temperature observation cavity with a micro-area representation function and an operation method, wherein the portable ultrahigh vacuum low-temperature observation cavity comprises an ultrahigh vacuum main cavity with a multi-port tubular structure, and the cavity is communicated with a sample transfer rod, an air suction pump, a hand valve, a corrugated pipe and a glass observation window; a cold cavity extending into the ultrahigh vacuum main cavity is arranged in the corrugated pipe, and a sample storage groove for placing a UHV sample support handle is arranged at the outer end part of the cold cavity; and the sample transfer rod extends into the ultrahigh vacuum main cavity, and the UHV sample is conveyed into a sample storage rack for long-term storage, or the UHV sample is conveyed into a sample storage groove for optical observation, or the UHV sample is transferred to other ultrahigh vacuum devices. According to the invention, the sample is kept at an ultralow temperature state, and meanwhile, the air suction pump ensures that the sample is always in an ultrahigh vacuum environment, the corrugated pipe is adjusted to realize the axial movement of the sample storage groove, the distance between the sample and the glass observation window is adjusted to enable the sample to be close enough, and the complex optical characteristics of large-angle observation, micro-area observation and the like of the sample are realized.
Description
Technical Field
The invention belongs to the field of ultrahigh vacuum equipment, and particularly relates to a portable ultrahigh vacuum low-temperature observation cavity with a micro-area representation function and an operation method thereof.
Background
Ultra-high vacuum systems (UHV) have found wide application in various research fields, including semiconductor, machining, physics, chemistry, materials and bioscience. The material prepared by the UHV system (hereinafter referred to as UHV material) has high quality, less impurities and high scientific research value. However, the surface of the UHV material is sensitive, and the requirements on vacuum degree and temperature are high. Therefore, after the sample is prepared in the ultra-high vacuum system, in order to ensure the stable properties of the sample, structural characterization and optical analysis are generally required in an environment without destroying the ultra-high vacuum.
At present, the cryogenic optical thermostat devices are roughly classified into 2 types, wherein one type of the devices is characterized by having a well-designed optical path and a large window, and being capable of realizing high-requirement cryogenic optical analysis, such as micro-area characterization at liquid helium temperature, and having the defects of large volume and immobility; the other type is relatively portable and has good low temperature performance, but the sample position is fixed and is far away from the glass observation window, so that the capability of micro-area characterization is limited. Furthermore, neither type is specifically designed for UHV environments, and neither type is used for ultra-high vacuum samples to avoid the "open cavity sampling" procedure, which necessarily results in exposure of the sample to atmospheric conditions. In this process, the external gas is adsorbed to the surface of the sample, and the sample is contaminated to some extent.
At present, no observation cavity device which has a good light path design with micro-area and large-angle observation capability and better portability and can ensure low-temperature storage conditions in the carrying process on the premise of not damaging the ultra-high vacuum environment of the UHV sample exists.
Disclosure of Invention
In order to solve the above-mentioned defects in the prior art, the present invention aims to provide a portable ultra-high vacuum low temperature observation chamber with a micro-area characterization function and an operation method thereof. On the premise of ultra-high vacuum and ultra-low temperature standards, a sample transfer cavity and a refrigerating liquid cavity are integrated. The cavity can realize the purpose of transferring the UHV sample on the premise of not damaging ultrahigh vacuum, has good light path design for micro-area observation and large-angle observation of the UHV sample, has better portability and can ensure that the UHV sample is always kept in an ultrahigh vacuum and ultralow temperature environment in the carrying process. The invention is realized by the following technical scheme.
The invention is realized by the following technical scheme.
A portable ultrahigh vacuum low-temperature observation cavity with a micro-area representation function comprises an ultrahigh vacuum main cavity body with a multi-opening tubular structure, wherein a sample transfer rod is communicated with the front wall of the ultrahigh vacuum main cavity body, and an air suction pump is communicated with the lower part of the same side of the sample transfer rod; the rear wall is communicated with a hand valve, the right wall is communicated with a corrugated pipe, and the left wall is provided with a glass observation window;
the lower end of the sample storage rod is connected with a sample storage rack extending into the ultrahigh vacuum main cavity, a cold cavity extending into the ultrahigh vacuum main cavity is arranged in the corrugated pipe, and a sample storage groove for placing a UHV sample support handle is arranged at the outer end part of the cold cavity; and the sample transfer rod extends into the ultrahigh vacuum main cavity, and the UHV sample is conveyed into a sample storage rack for long-term storage, or the UHV sample is conveyed into a sample storage groove for optical observation, or the UHV sample is transferred to other ultrahigh vacuum devices.
With respect to the above technical solutions, the present invention has a further preferable solution:
preferably, the cold cavity comprises an inner layer and an outer layer which are respectively communicated with the outside or the refrigerating liquid bin through an outer pipeline of the cold cavity extending outwards, and a sample storage groove is arranged at the inner end part of the outer layer of the cold cavity.
Preferably, the opening of the sample storage groove faces one side of the sample transfer rod, and a semicircular groove is formed in the opening.
Preferably, the side wall of the inner layer of the cold cavity close to the sample storage groove is provided with a small hole, the outer layer pipeline of the cold cavity is connected to the inner diameter of the sealing flange at the end part of the corrugated pipe, and the cold cavity can axially move along with the expansion of the corrugated pipe.
Preferably, the sample transfer rod is communicated with a sampling head extending into the main cavity; the sampling head is provided with a rectangular groove which is butted with the UHV sample support handle.
Preferably, one end of the hand valve is connected with the main cavity in a sealing mode through a flange, and the other end of the hand valve is provided with a sealing interface for connecting other ultrahigh vacuum systems.
Preferably, the distance between the UHV sample and the objective or other observation device is at least 0.5 mm.
Preferably, the sample storage rod is connected with the ultrahigh vacuum main cavity through a sealing flange and moves up and down, the lower end of the sample storage rod is connected with a sample storage rack, the sample storage rack is provided with a plurality of layers, and each layer can contain one UHV sample.
The invention further provides an operation method of the portable ultrahigh vacuum low-temperature observation cavity, which comprises the following steps:
UHV sample transfer:
the interior of the ultrahigh vacuum main cavity is in an ultrahigh vacuum state, the ultrahigh vacuum main cavity is hermetically connected with a target ultrahigh vacuum device through a hand valve, and an axially telescopic sample transfer rod extends into the target ultrahigh vacuum device to grab a UHV sample;
retracting the sample transferring rod to the sampling head and returning the sampling head to the ultrahigh vacuum main cavity;
axially moving the corrugated pipe to enable the sample storage groove and the sampling head to be positioned on the same plane, conveying the UHV sample fixed on the sampling head into the sample storage groove or the sample storage rack, isolating the ultrahigh vacuum main cavity from the target ultrahigh vacuum device, and removing the target ultrahigh vacuum device;
repeating the operation, and conveying a plurality of UHV samples into a sample storage rack;
optical observations were made on UHV samples:
and for the UHV sample transferred into the sample storage groove, axially moving the corrugated pipe to enable the UHV sample to be close to the optical observation window, moving the corrugated pipe to adjust the distance between the sample and the optical measurement device, and placing the ultrahigh vacuum main cavity with the UHV sample on an optical platform exposed in the atmosphere to perform optical measurement at different focal lengths.
Preferably, the UHV sample is optically measured by Raman spectroscopy, X-ray diffraction measurement, micro-area observation or large-angle observation under the ultra-high vacuum and ultra-low temperature environment.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
according to the invention, the refrigeration medium is injected into the cold cavity, so that the sample is kept in an ultralow temperature state, and meanwhile, the suction pump ensures that the sample is always in an ultrahigh vacuum environment. The corrugated pipe is adjusted to realize axial movement of the sample storage groove, the distance between the sample and the glass observation window is adjusted to enable the sample to be close enough, and complex optical characteristics such as large-angle observation, micro-area observation and the like of the sample are realized. The micro-area and large-angle optical characterization function of the UHV sample can be realized under the condition of not damaging ultrahigh vacuum, the combination design of the cold cavity and the observation cavity ensures that the UHV sample has good portability and ensures the low-temperature condition in the carrying process, and an integrated solution is provided for the transfer storage, the optical characterization and the carrying of the UHV sample.
The observation cavity can adjust the distance from the glass observation window through the telescopic pipeline, so that a sample can be close to the inner surface of the observation window enough for focusing, the observation cavity actively adapts to the light path of external optical observation equipment, and optical characterization with high requirements such as large angle, micro-area and the like can be carried out.
In the invention, the cold cavity Dewar design capable of axially moving back and forth, and the corresponding sample groove and the optical observation window design form a horizontal light path observation system, so that on one hand, the difficulty of light path configuration is reduced, and the system has stronger applicability compared with the traditional light path observation in the vertical direction; on the other hand, the horizontal design can enable the sample to be close to the observation window enough, and the micro-area characterization function which is difficult to achieve by a vertical light path is realized.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is a schematic view of the external overall structure of the portable ultra-high vacuum low temperature observation chamber with micro-area characterization function according to the present invention;
FIG. 2, FIG. 3 and FIG. 4 are schematic cross-sectional views of the portable ultra-high vacuum low temperature observation chamber with micro-area characterization function for sample transfer;
FIG. 5 is a sectional view of a cold chamber of the portable ultra-high vacuum low temperature observation chamber with a micro-area characterization function according to the present invention during optical observation;
FIG. 6 is an external schematic view of the portable ultra-high vacuum low-temperature observation cavity with micro-area characterization function according to the present invention during optical measurement.
Reference numerals: 1. an ultra-high vacuum main chamber; 2. a bellows; 3. a sample transfer rod; 4. a getter pump; 5. a glass viewing window; 6. a hand valve; 7. a sample storage rod; 21. UHV samples; 22. a sample storage groove; 23. a semicircular groove; 24. a sampling head; 25. a sample storage rack; 31. an inner layer of the cold chamber; 32. an outer layer of the cold chamber; 33. a small hole; 34. a cold chamber inner layer conduit; 35. a cold chamber outer layer pipeline; 41. an objective lens or other viewing device.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
Referring to fig. 1 and 2, the portable ultrahigh vacuum low-temperature observation cavity with the micro-area characterization function has a main structure comprising an ultrahigh vacuum main cavity 1, a corrugated pipe 2, a sample transfer rod 3, an air suction pump 4, a glass observation window 5, a hand valve 6, a sample storage rod 7, a sample storage rack 25 and a cold cavity.
Referring to fig. 1, an ultrahigh vacuum main cavity 1 is in a multi-port tubular structure and is made of high-strength materials (such as stainless steel), so that the ultimate vacuum in the cavity can meet the ultrahigh vacuum requirement; the welding has 6 sealed flanges on the super high vacuum main cavity body 1, and the antetheca intercommunication has a biography appearance pole 3, and the flange intercommunication of 3 homonymy belows in biography appearance pole has aspirator pump 4, and the back wall intercommunication has hand valve 6, and the right wall has bellows 2 through the flange intercommunication, and the left wall is equipped with glass observation window 5, and the upper wall intercommunication has a sample storage pole 7, and sample storage frame 25 is connected to sample storage pole 7 lower extreme, and sample storage frame stretches into inside the super high vacuum main cavity body 1.
The left wall of the corrugated pipe 2 is butted with a flange on the wall surface of the ultrahigh vacuum main cavity 1, and the right wall is connected with a sealing flange. The double-layer refrigerating liquid pipeline penetrates through the sealing flange, and the inner wall of the sealing flange is welded with the outer wall of the cold cavity pipeline. The corrugated pipe 2 can move in an axial telescopic way, so that the cold cavity is driven to move in an axial direction.
Referring to fig. 1 and 2, one end of a sample transfer rod 3 is communicated with an ultrahigh vacuum main cavity 1 through a flange and can rotate and axially move in a telescopic manner; one end of the sample transmission rod 3 is provided with a sampling head 24 extending into the ultrahigh vacuum main cavity 1; a sample storage groove 22 extending into the ultrahigh vacuum main cavity 1 is arranged in the corrugated pipe 2, and a UHV sample 21 is placed in the sample storage groove 22; the sampling head 24 is provided with a rectangular recess which interfaces with the holder of the UHV sample 21. The UHV sample 21 support handle is in butt joint with the sampling head 24, the UHV sample 21 is grabbed and loosened by the sampling head 24 through rotating the sample transfer rod 3, and the UHV sample 21 is sent into or moved out of the sample storage groove or the sample storage rack through the telescopic sample transfer rod.
Referring to fig. 1 and 2, the getter pump 4 below the ultra-high vacuum main chamber 1 on the same side as the sample transfer rod 3 is communicated with the ultra-high vacuum main chamber 1 through a sealing flange, and the getter pump 1 is always in a working state to maintain the ultra-high vacuum state inside the ultra-high vacuum main chamber 1.
Referring to fig. 1, 2 and 6, the glass observation window 5 is arranged at the other side opposite to the corrugated pipe 2 on the ultrahigh vacuum main cavity 1, the glass observation window 5 is communicated with the ultrahigh vacuum main cavity 1 through a sealing flange, and the glass observation window 5 adopts an ultrahigh vacuum pure quartz observation window with an antireflection film, so that high light transmittance is ensured during optical measurement, optical signal loss in the measurement process is reduced, and interference of optical noise is eliminated as much as possible. Thanks to the design of movable bellows 2, UHV sample 21 can be closely attached without touching glass window 5, and glass window 5 can be as thin as 0.5mm in thickness, so that UHV sample 21 is spaced from objective lens or other observation device 41 by a minimum of 0.5mm, and micro-area observation and large-angle observation of UHV sample 21 can be realized.
Referring to fig. 1 and 2, the hand valve 6 is arranged on a flange communicated with the ultrahigh vacuum main cavity 1 on the opposite side of the sample transfer rod 3, one end of the hand valve 6 is communicated with the ultrahigh vacuum main cavity 1 through a sealing flange, and the other end is provided with a sealing interface butted with other ultrahigh vacuum systems. When the ultrahigh vacuum system is in butt joint with other ultrahigh vacuum systems, the sealing interface is firstly in butt joint with the target ultrahigh vacuum system interface, and then the hand valve is rotated to communicate the ultrahigh vacuum main cavity 1 with the system, so that the UHV sample is taken and placed, and the sample is ensured to be in an ultrahigh vacuum environment in the whole process. After sampling, the hand valve 6 is rotated to close the internal passage, and then the ultrahigh vacuum device is removed.
Referring to fig. 1, 2, 4 and 5, the sample storage rod 7 is connected to the ultra-high vacuum main chamber 1 through a sealing flange, and the lower end thereof is connected to the sample storage rack 25. The sample holder 25 is provided with 5 layers, each layer being adapted to hold one UHV sample 21. The sample storage rod 7 can move up and down, thereby driving the sample storage rack 25 to move up and down in the ultrahigh vacuum main cavity 1. It can be understood that the UHV sample can be sent to the sample storage rack 25 for long-term storage by connecting the hand valve 6 with other ultrahigh vacuum devices and operating the sample transfer rod 3 and the sample storage rod 7, and the UHV sample on the sample storage rack 25 can also be transferred to other ultrahigh vacuum devices. Further, the UHV sample on the sample storage rack 25 can be sent to the sample storage groove 22 for optical observation or the UHV sample 21 in the sample storage groove 22 can be sent to the sample storage rack 25 for storage by operating the transfer rod 3 and the sample storage rod 7.
Referring to fig. 3 and 5, the cold cavity is located in the corrugated pipe 2 and is divided into a cold cavity inner layer 31 and a cold cavity outer layer 32, one end of the cold cavity inner layer 31 is provided with a cold cavity inner layer pipeline 34 extending outwards, the same end of the cold cavity outer layer 32 is provided with a cold cavity outer layer pipeline 35 coaxial with the cold cavity inner layer pipeline 34 and slightly thicker, the outer wall of the other end of the cold cavity is provided with a sample storage groove 22 and a semicircular groove 23, the designed sample storage groove 22 can contain a UHV sample holder, and the designed semicircular groove 23 can be in butt joint with a sampling head 24. The cold cavity inner layer 31 is communicated with the cold cavity outer layer 32 through a round small hole 33, and the round small hole 33 is close to the sample storage groove 22. The cold chamber inner layer pipe 34 is connected with a container filled with refrigerant, and the refrigerant is injected into the cold chamber, wherein the injection amount is determined according to the specific conditions of the experiment (the maximum capacity is 125 ml). The refrigerant absorbs heat and is gasified in the cold cavity inner layer 31, and then escapes to the cold cavity outer layer 32 through the round small hole 33, and is discharged outside through the cold cavity outer layer pipeline 35. The outer layer pipeline 35 of the cold cavity is welded with the corrugated pipe 2 at the inner diameter of the sealing flange, so that the cold cavity can axially move along with the expansion of the corrugated pipe, the UHV sample 21 in the sample storage groove 22 axially moves, and the distance between the UHV sample 21 and the glass observation window 5 is adjusted.
The components ensure that UHV samples of other ultrahigh vacuum systems can be transferred to the invention for long-term storage or long-distance transportation under the condition of not damaging ultrahigh vacuum, and the invention can store 6 UHV samples at the same time; furthermore, the invention can realize high-quality optical measurement (such as micro-area observation and angle amplification observation) on the UHV sample in the ultra-high vacuum and ultra-low temperature environment.
The specific operation flow of the portable ultra-high vacuum low-temperature observation cavity with the micro-area characterization function for transferring the UHV sample and optically observing the UHV sample is described in detail below with reference to FIGS. 1 to 6.
A. UHV sample transfer was performed:
firstly, communicating an ultrahigh vacuum main cavity with a target ultrahigh vacuum device through a hand valve 6, simultaneously operating a vacuumizing device and an air suction pump to enable the interior of the ultrahigh vacuum main cavity to reach an ultrahigh vacuum state, ensuring that two ends of the hand valve 6 belong to ultrahigh vacuum magnitude, and opening the hand valve to enable the ultrahigh vacuum main cavity to be communicated with the target ultrahigh vacuum device; then an axially telescopic sample transfer rod 3 extends into a target ultrahigh vacuum device to grab a UHV sample, a sample head wraps a UHV sample support, and the sample transfer rod is rotated to fix the UHV sample support on the sample transfer rod; the retraction of the transfer rod 3 enables the sampling head to avoid the sample storage tank 22 or the sample storage rack 25, retracting the transfer rod until the sampling head returns to the ultra-high vacuum main chamber and can not be retracted any further. And moving the corrugated pipe 2 or the sample storage rack 25 downwards to enable a layer of the sample storage groove 22 or the sample storage rack 25 to be aligned with the sampling head 24, axially extending the sample transfer rod 3 to enable the UHV sample holder to approach the sample storage groove 22, finely adjusting the corrugated pipe 2 to enable the sample storage groove 22 to be aligned with the UHV sample holder, continuously extending the sample transfer rod, continuously operating the sample transfer rod 3 to send the UHV sample into the sample storage groove 22 or the sample storage rack 25, rotating the sample transfer rod to enable the UHV sample holder to be separated from the sampling head, and retracting the sampling rod. The hand valve is closed to isolate the two devices, and the ultra-high vacuum device is removed.
When the transfer rod 3 or the rack 25 is manipulated, the position thereof can be observed through the glass observation window 5. It will be appreciated that the above operations are performed in reverse order and that UHV sample 21 may be transferred to other ultra-high vacuum devices.
The operation can transfer one or more UHV samples in one ultrahigh vacuum system to a sample storage groove or a sample storage rack of the ultrahigh vacuum main cavity by using the sample transfer device under the condition of not contacting with the external air for optical observation or low-temperature storage, and also transfer the UHV samples to another ultrahigh vacuum system under the condition of not contacting with the external air.
When optical observation is performed (UHV sample 21 is present in the sample well 22), the sample holder 25 is first raised, the transfer rod 3 is retracted, and the bellows 2 is then pushed until the UHV sample 21 is in close proximity to, but not touching, the glass window 5. And then transferring the portable ultra-high vacuum low-temperature observation cavity with the UHV sample and the micro-region characterization function to an atmospheric optical platform for optical measurement. Bellows 2 can continue to be adjusted during the measurement to adjust the distance between UHV sample 21 and objective lens or other optical measurement device 41 to accommodate optical observations at different focal lengths. The refrigeration medium in the cold chamber can maintain the ultra-low temperature state of the UHV sample 21 for a period of time, and if the UHV sample needs to be researched under a plurality of research devices, the ultra-high vacuum main chamber body 1 with the UHV sample can be moved to different devices for observation in the period of time until the research is completed.
The operation can realize high-quality optical measurement of the sample in an ultra-high vacuum and ultra-low temperature environment.
In conclusion, the portable ultrahigh vacuum low-temperature observation cavity with the micro-area representation function, which is designed by the invention, realizes the transfer and storage of UHV samples among different ultrahigh vacuum systems on the premise of not damaging an ultrahigh vacuum environment; the optical observation of the UHV sample under the ultra-high vacuum and ultra-low temperature environment is realized. The whole process keeps the surface of the sample clean and ensures the accuracy of the observation result. Meanwhile, all the ultrahigh vacuum equipment are not mechanically connected, so that mutual interference among the ultrahigh vacuum equipment is effectively avoided, and the equipment is simple and convenient to operate, short in time consumption, low in cost, suitable for various observation means and high in use and popularization values.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (10)
1. A portable ultrahigh vacuum low-temperature observation cavity with a micro-area representation function is characterized by comprising an ultrahigh vacuum main cavity body with a multi-opening tubular structure, wherein the front wall of the ultrahigh vacuum main cavity body is communicated with a sample transfer rod, and the lower parts of the same side of the sample transfer rod are communicated with an air suction pump; the rear wall is communicated with a hand valve, the right wall is communicated with a corrugated pipe, and the left wall is provided with a glass observation window;
the lower end of the sample storage rod is connected with a sample storage rack extending into the ultrahigh vacuum main cavity, a cold cavity extending into the ultrahigh vacuum main cavity is arranged in the corrugated pipe, and a sample storage groove for placing a UHV sample support handle is arranged at the outer end part of the cold cavity; and the sample transfer rod extends into the ultrahigh vacuum main cavity, and the UHV sample is conveyed into a sample storage rack for long-term storage, or the UHV sample is conveyed into a sample storage groove for optical observation, or the UHV sample is transferred to other ultrahigh vacuum devices.
2. The portable ultrahigh vacuum low-temperature observation chamber with the micro-area characterization function as claimed in claim 1, wherein the cold chamber comprises an inner layer and an outer layer, the inner layer and the outer layer are respectively communicated with the outside or a refrigerating liquid bin through an outer layer pipeline of the cold chamber extending outwards, and a sample storage groove is formed in the inner end part of the outer layer of the cold chamber.
3. The portable ultra-high vacuum low temperature observation chamber with the micro-area characterization function as claimed in claim 2, wherein the sample storage groove has an opening facing one side of the sample transfer rod, and a semicircular groove is formed at the opening.
4. The portable ultra-high vacuum low temperature observation chamber with the micro-area characterization function as claimed in claim 2, wherein the inner wall of the cold chamber close to the sample storage groove is provided with small holes, the outer pipe of the cold chamber is connected to the inner diameter of the sealing flange at the end of the corrugated pipe, and the cold chamber can move axially along with the expansion of the corrugated pipe.
5. The portable ultrahigh vacuum low temperature observation chamber with the micro-area characterization function of claim 1, wherein the sample transfer rod is communicated with a sampling head extending into the main chamber; the sampling head is provided with a rectangular groove which is butted with the UHV sample support handle.
6. The portable ultrahigh vacuum low-temperature observation chamber with the micro-region characterization function as claimed in claim 1, wherein one end of the hand valve is connected with the main chamber body through a flange in a sealing manner, and the other end of the hand valve is provided with a sealing interface for connecting other ultrahigh vacuum systems.
7. The portable ultra-high vacuum low temperature observation chamber with the micro-area characterization function of claim 1, wherein the distance between the UHV sample and the objective lens or other observation devices is at least 0.5 mm.
8. The portable ultra-high vacuum low temperature observation chamber with the micro-region characterization function as claimed in claim 1, wherein the sample storage rod is connected with the ultra-high vacuum main chamber through a sealing flange, moves up and down, the lower end of the sample storage rod is connected with a sample storage rack, the sample storage rack is provided with a plurality of layers, and each layer can contain one UHV sample.
9. A method of operating a cryoscope based on any of claims 1 to 8, comprising:
UHV sample transfer:
the interior of the ultrahigh vacuum main cavity is in an ultrahigh vacuum state, the ultrahigh vacuum main cavity is hermetically connected with a target ultrahigh vacuum device through a hand valve, and an axially telescopic sample transfer rod extends into the target ultrahigh vacuum device to grab a UHV sample;
retracting the sample transferring rod to the sampling head and returning the sampling head to the ultrahigh vacuum main cavity;
axially moving the corrugated pipe to enable the sample storage groove and the sampling head to be positioned on the same plane, conveying the UHV sample fixed on the sampling head into the sample storage groove or the sample storage rack, isolating the ultrahigh vacuum main cavity from the target ultrahigh vacuum device, and removing the target ultrahigh vacuum device;
repeating the operation, and conveying a plurality of UHV samples into a sample storage rack;
optical observations were made on UHV samples:
and for the UHV sample transferred into the sample storage groove, axially moving the corrugated pipe to enable the UHV sample to be close to the optical observation window, moving the corrugated pipe to adjust the distance between the sample and the optical measurement device, and placing the ultrahigh vacuum main cavity with the UHV sample on an optical platform exposed in the atmosphere to perform optical measurement at different focal lengths.
10. The method of claim 9, wherein the UHV sample is optically measured in an ultra-high vacuum, ultra-low temperature environment using raman spectroscopy, X-ray diffraction measurements, micro-field observation, or high angle observation.
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| CN116087102A (en) * | 2023-01-13 | 2023-05-09 | 中国科学院空间应用工程与技术中心 | Experimental device for ice satellite and open-sea ocean extreme environment simulation system |
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