CN114813735B - Ultrahigh vacuum extremely-low temperature nano material preparation and characterization equipment - Google Patents

Ultrahigh vacuum extremely-low temperature nano material preparation and characterization equipment Download PDF

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CN114813735B
CN114813735B CN202210396230.9A CN202210396230A CN114813735B CN 114813735 B CN114813735 B CN 114813735B CN 202210396230 A CN202210396230 A CN 202210396230A CN 114813735 B CN114813735 B CN 114813735B
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cavity
preparation
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ultra
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CN114813735A (en
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张宇
马诚杰
沈敏敏
王城程
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Yisheng Scientific Instrument Jiaxing Co ltd
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Yisheng Scientific Instrument Jiaxing Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

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Abstract

The invention provides ultrahigh vacuum extremely-low temperature nano-material preparation and characterization equipment, which aims to solve the problems that the existing nano-material measurement device can only realize measurement by a single technical means and cannot provide an extremely-low temperature environment, and meanwhile, a plurality of influence factors exist when nano-material is transferred in an atmospheric environment after being prepared, and the equipment comprises a supporting device used as an installation substrate, and also comprises: the electric cabinet is used for integrated control of electric elements in the equipment; the interconnection channel is used for integrating the equipment into the workstation so as to transmit the prepared nano material to the next procedure for in-situ measurement; the top end of the supporting device is provided with a rapid sample introduction device, a sample preparation device and a sample measurement device which are connected in sequence. The method is particularly suitable for systematic preparation and characterization of the nano material in an ultra-high vacuum and extremely-low temperature environment, and has high social use value and application prospect.

Description

Ultrahigh vacuum extremely-low temperature nano material preparation and characterization equipment
Technical Field
The invention relates to the technical field of nano materials, in particular to preparation and characterization equipment of an ultrahigh vacuum extremely-low temperature nano material.
Background
The characterization of the nanometer material mainly aims to determine some physical and chemical characteristics of the nanometer material, such as morphology, size, particle size, isoelectric point, chemical composition, crystal structure, forbidden bandwidth, light absorption characteristic and the like. At present, various technical means can realize the characterization of the nano material, however, the measuring devices adopted by different technical means are often not universal, and each measuring device can only realize the measurement of a single technical means, which hinders the development of the material characterization technology and the development of related scientific research.
Meanwhile, the extremely low temperature region is one of the most important extreme physical experimental conditions, can inhibit random thermal motion of electrons, atoms and the like in substances, shows the advantages of pure quantum mechanical phenomena and the like, and is more and more emphasized by the technical field of material characterization. The existing nano material measuring device can only realize the measurement by a single technical means, cannot provide an extremely low temperature environment, simultaneously needs to be independently prepared, and has a plurality of influence factors in the process of transferring to measuring equipment in an atmospheric environment. Therefore, an ultrahigh vacuum extremely-low temperature nano material preparation and characterization device is provided.
Disclosure of Invention
It is an object of the present invention to solve or at least alleviate problems in the prior art.
In order to achieve the purpose, the invention is realized by the following technical scheme: the preparation and characterization equipment of the ultra-high vacuum extremely-low temperature nano material comprises a supporting device used as an installation base body and further comprises: the electric cabinet is used for integrated control of electric elements in the equipment; the interconnection channel is used for integrating the equipment into the workstation so as to transmit the prepared nano material to the next procedure for in-situ measurement;
the top of the supporting device is provided with a rapid sample introduction device, a sample preparation device and a sample measurement device which are connected in sequence:
the rapid sample introduction device is used for rapidly replacing samples and consumable accessories in equipment in an ultrahigh vacuum state;
the sample preparation device is used for preparing the nano material in an ultrahigh vacuum state and transferring the prepared nano material to the sample measurement device;
the sample measuring device is used for characterization of the nano material under the ultra-high vacuum extremely-low temperature environment and transferring the nano material to the interconnection channel.
Optionally, the supporting device includes a supporting frame and a panel disposed on the supporting frame, and the supporting frame is composed of an aluminum frame and stainless steel supporting columns.
Optionally, the rapid sampling device is provided with a sample cavity on the supporting device, and the sample cavity is provided with:
a first quick-open door for feeding the sample and consumable accessories in the apparatus;
a first pair of interfaces for interfacing with a sample preparation device;
the first sample transfer control rod is used for realizing mutual transfer of the sample and the consumable fittings in the equipment between the sample feeding cavity and the sample preparation device.
Optionally, the sample preparation device includes a preparation cavity disposed at the upper end of the supporting device and a transmission cavity communicated with the preparation cavity, the transmission cavity is provided with a second pair of interfaces butted with the first pair of interfaces, and the preparation cavity is provided with:
a third docking interface for docking with a sample measurement device;
the sample stage assembly is used for fixing a sample and controlling the angle in an ultrahigh vacuum state;
the evaporation assembly and the etching assembly are used for preparing nano materials with different shapes;
a first microscopic observation assembly for observing the sample stage assembly from right below;
the second microscopic observation assembly is used for observing the sample stage assembly from the right front side;
the third sample transfer control rod is used for realizing mutual transfer of the sample and consumable accessories in the equipment between the rapid sample introduction device and the transmission cavity;
and the second sample transmission control rod is used for preparing the nano material and transmitting the nano material between the preparation cavity and the sample measuring device.
Optionally, the preparation chamber and the transmission chamber are respectively provided with a plurality of first observation windows for observing the transmission state of the sample.
Optionally, the sample stage assembly comprises:
the sample pedestal is used for sample fixation and nano-scale precision angle control;
the mask plate seat is used for preparing mask plate fixing and nano-scale precision angle control by nano materials;
the large-range moving part is used for realizing XYZ-axis and rotation four-dimensional movement of the sample pedestal and the mask plate pedestal.
Optionally, the sample measuring device includes a measuring cavity disposed at an upper end of the supporting device, the measuring cavity has a measuring head for characterizing the nano material, and the measuring cavity is provided with:
a fourth docking port for docking with the third docking port;
a fifth sample transfer lever for preparing the nanomaterial to be transferred between the measurement cavity and the sample preparation device;
a helium tri-refrigerator for refrigerating the measurement cavity and maintaining a very low temperature environment;
the superconducting magnet is used for generating a magnetic field without energy loss when operating under the condition of direct current;
the cold screen is used for reducing heat radiation heat leakage of the measuring head;
and the third microscopic observation assembly is used for transmitting the cold shield and the superconducting magnet and performing optical interaction with the measuring head.
Optionally, the first pair of interfaces, the second pair of interfaces, the third pair of interfaces, the fourth pair of interfaces, and the fifth pair of interfaces are respectively provided with a flexible bellows for ensuring flexible connection of the devices and an ultrahigh vacuum gate valve for selectively opening or closing the channel.
Optionally, the measurement cavity is communicated with a sample transfer cavity through a sample transfer assembly, a fifth interface communicated with the interconnection channel is arranged on the sample transfer cavity, and a fourth sample transfer control rod used for realizing mutual transfer of the prepared nano material between the sample transfer cavity and the interconnection channel is arranged on the sample transfer cavity.
Optionally, the rapid sampling device, the sample preparation device and the sample measurement device are all provided with an ultrahigh vacuum obtaining and measuring assembly, and the ultrahigh vacuum obtaining and measuring assembly comprises a vacuum pump set for vacuumizing the inside of the cavity to obtain an ultrahigh vacuum state, a vacuum plate valve for closing an upper opening of the cavity to maintain the ultrahigh vacuum state inside the cavity, and a vacuum gauge for detecting the ultrahigh vacuum state inside the cavity.
The embodiment of the invention provides a device for preparing and characterizing an ultrahigh vacuum extremely-low temperature nano material, which has the following beneficial effects:
1. the ultrahigh vacuum state in the rapid sample introduction device, the sample preparation device and the sample measurement device is ensured through the ultrahigh vacuum obtaining and measuring component, wherein sample materials and easily-consumed accessories (such as a mask plate, a probe and the like) in equipment are sent from the rapid sample introduction device and transferred to the sample preparation device in the ultrahigh vacuum state, the measurement time and the measurement cost are saved, the sample preparation device is used for preparing and processing the nano materials for the sample, and after the preparation processing is finished, the nano materials are sent to the sample measurement device to be used for representing the nano materials in the ultrahigh vacuum extremely-low temperature environment.
2. According to the invention, the shape and the size precision of the nano material sample required by preparation can be judged more intuitively and accurately by arranging the first microscopic observation assembly and the second microscopic observation assembly on the preparation cavity, and the sample pedestal can be selectively and additionally provided with heating parts such as thermal radiation heating, electron bombardment heating or direct current heating, so that the nano material sample with better performance can be prepared.
3. The sample measuring device realizes the nano material characterization of various technical means in the same set of equipment by replacing the measuring head assembly in the ultrahigh vacuum extremely-low temperature environment, and can be compatible with various technical means such as STM, AFM, MFM, SNOM, transport measurement and the like to realize the in-situ nano material characterization.
4. The flexible corrugated pipe for ensuring flexible connection and the ultrahigh vacuum gate valve for selectively opening or closing the channel are arranged on the butt joint interface of each device, so that the flexible connection between two butted devices can be ensured while the butt joint and intercommunication function is realized, the channel is selectively opened or closed, and the mutual influence between the two devices is reduced.
Drawings
The above features, technical features, advantages and implementation manners of an ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device will be further described in the following detailed description of preferred embodiments with reference to the accompanying drawings.
FIG. 1 is a schematic perspective view of the present invention;
FIG. 2 is a front view of the present invention;
FIG. 3 is a perspective view of the supporting device of the present invention;
FIG. 4 is a perspective view of the rapid sampling device of the present invention;
FIG. 5 is a perspective view of a sample preparation device according to the present invention;
FIG. 6 is an exploded view of the structure of a sample preparation device according to the present invention;
FIG. 7 is a perspective view of a sample measuring device according to the present invention;
FIG. 8 is a side view of the construction of a sample measuring device according to the present invention;
FIG. 9 isbase:Sub>A schematic view of the structure A-A shown in FIG. 8 according to the present invention.
In the figure: an electric cabinet 10, a supporting device 20, a rapid sample introduction device 30, a sample introduction cavity 300, a first rapid opening door 301, a first pair of interfaces 302, a first sample transfer control rod 303,
The device comprises a sample preparation device 40, a preparation cavity 400, a transmission cavity 401, a sample stage assembly 402, a large-range motion member 421, a sample stage 422, a mask plate seat 423, a second interface 403, a first observation window 405, a third interface 406, an evaporation assembly 407, an etching assembly 408, a first microscopic observation assembly 409, a second microscopic observation assembly 410, a second sample transmission control rod 411, a third sample transmission control rod 412, a sample measurement device 50, a measurement cavity 500, a measurement head 511, a fourth interface 501, a sample transfer assembly 502, a sample transfer cavity 503, a fifth interface 531, a fourth sample transmission control rod 504, a fifth sample transmission control rod 505, a second observation window 506, a helium three refrigerator 507, a third microscopic observation assembly 508, a superconducting magnet 509, a cold shield 510, a sample holder,
The system comprises an interconnection channel 60, an ultrahigh vacuum obtaining and measuring assembly 70, a vacuum pump group 701, a vacuum plate valve 702, a vacuum gauge 703 and an expansion flange port 80.
Detailed Description
The invention will be further illustrated with reference to the following figures 1 to 9 and examples:
example 1
An ultra-high vacuum ultra-low temperature nano material preparation and characterization device, referring to the attached fig. 1-3, comprising a supporting device 20 as an installation base body, and further comprising: the electric cabinet 10 is used for integrated control of electric elements in the equipment; an interconnect channel 60 for device integration to the workstation for transporting the prepared nanomaterial to the next process for in situ measurement;
the top end of the supporting device 20 is provided with a rapid sampling device 30, a sample preparation device 40 and a sample measuring device 50 which are connected in sequence:
the rapid sample introduction device 30 is used for rapidly replacing samples and consumable accessories in equipment in an ultrahigh vacuum state, so that the measurement time and the cost are saved;
the sample preparation device 40 is used for preparing the nano material in an ultrahigh vacuum state and transferring the prepared nano material to the sample measurement device 50;
the sample measuring device 50 is used for characterization of the nano material under the ultrahigh vacuum extremely-low temperature environment and transferring the nano material to the interconnection channel 60;
the rapid sampling device 30, the sample preparation device 40 and the sample measurement device 50 are all provided with an ultrahigh vacuum obtaining and measuring assembly 70, and the ultrahigh vacuum obtaining and measuring assembly 70 comprises a vacuum pump group 701 for vacuumizing the inside of the cavity to obtain an ultrahigh vacuum state, a vacuum plate valve 702 for closing an upper opening of the cavity to maintain the ultrahigh vacuum state inside the cavity, and a vacuum gauge 703 for detecting the ultrahigh vacuum state inside the cavity;
in the application, the ultrahigh vacuum obtaining and measuring component 70 ensures the ultrahigh vacuum state inside the rapid sampling device 30, the sample preparation device 40 and the sample measuring device 50, wherein the sample material and the consumable parts (such as a mask, a probe and the like) in the device are sent from the rapid sampling device 30 and transferred to the sample preparation device 40 in the ultrahigh vacuum state, so that the measuring time and cost are saved, the sample preparation device 40 prepares and processes the sample with the nano material, after the preparation process is completed, the nano material is sent to the sample measuring device 50 to perform characterization of the nano material in the ultrahigh vacuum extremely low temperature environment, the selectable nano material is output to the interconnection channel 60 after the measurement characterization data is obtained, and is transmitted to the next procedure to perform in-situ measurement.
In this embodiment, as shown in fig. 1 to 3, the supporting device 20 includes a supporting frame 201 and a panel 202 disposed on the supporting frame, and the supporting frame 201 is composed of an aluminum frame and stainless steel supporting columns, and air floating legs, an optical bread board, stainless steel supporting columns and their combination may also be added to improve the damping performance of the apparatus.
In this embodiment, as shown in fig. 4, the rapid sample introduction device 30 includes a sample introduction cavity 300 disposed at the upper end of the supporting device 20, and the sample introduction cavity 300 is provided with:
a first quick-open door 301 for feeding samples and consumable accessories in the apparatus;
a first pair of interfaces 302 for interfacing with the sample preparation device 40;
a first sample transfer control rod 303 for realizing mutual transfer of the sample and consumable fittings in the device between the sample introduction cavity 300 and the sample preparation device 40;
in this embodiment, as shown in fig. 5 to 6, the sample preparation apparatus 40 includes a preparation chamber 400 disposed at the upper end of the supporting device 20 and a transmission chamber 401 communicated with the preparation chamber 400, the transmission chamber 401 is provided with a second pair of interfaces 403 butted with the first pair of interfaces 302, the preparation chamber 400 and the transmission chamber 401 are both provided with a plurality of first observation windows 405 for observing the transmission state of the sample, so as to conveniently observe the transmission state during sample transmission, and the preparation chamber 400 is provided with:
a third docking interface 406 for docking with the sample measurement device 50;
a sample stage assembly 402 for sample fixation and angle control in an ultra-high vacuum state;
wherein the sample stage assembly 402 comprises: the sample pedestal 422 is used for sample fixation and nano-scale precision angle control, in the embodiment, heating parts such as thermal radiation heating, electron bombardment heating or direct current heating and the like can be selectively added on the sample pedestal 422, so as to prepare a nano material sample with better performance; a mask plate seat 423 for mask plate fixing and nanometer precision angle control in nanometer material preparation; a large-range moving member 421 for realizing XYZ-axis and rotation four-dimensional movement of the sample holder 422 and the mask plate holder 423;
the evaporation assembly 407 and the etching assembly 408 are used for preparing nano materials with different shapes, in the embodiment, the evaporation assembly 407 can be a high-temperature evaporation source, a low-temperature evaporation source, an electron beam bombardment evaporation source and the like, and the etching assembly 408 can be an argon ion gun, so that sample preparation and processing means are enriched;
a first microscopic observation assembly 409 for observing the sample stage assembly 40 from right below, the first microscopic observation assembly 409 comprising a long-focus microscope, a reflector and a reflector driver to realize the observation of the sample stage assembly 40 from right below;
the second microscopic observation assembly 410 is used for observing the sample stage assembly 40 from the right front, and the second microscopic observation assembly 410 is a long-focus microscope and realizes the observation of the sample stage assembly 40 from the right front;
in this embodiment, the device further comprises an operation baffle assembly 413, which is used for simultaneously shielding and opening the first microscopic observation assembly 409 and the second microscopic observation assembly 410, so as to prevent the microscopic observation system from being polluted during sample preparation and influence the observation effect;
a third sample transfer control rod 412 for realizing mutual transfer of the sample and consumable fittings in the device between the rapid sample introduction device 30 and the transmission cavity 401;
a second sample transfer control rod 411 for transferring the prepared nanomaterial to and from the preparation chamber 400 and the sample measuring device 50;
in this embodiment, as shown in fig. 7-9, the sample measuring device 50 includes a measuring cavity 500 disposed on the upper end of the supporting device 20, a measuring head 511 for characterizing the nanomaterial is disposed in the measuring cavity 500, in this embodiment, the measuring head 511 may be an STM measuring head, an AFM measuring head, an MFM measuring head, an SNOM measuring head, a transportation measuring head, etc. to implement the nanomaterial characterization compatible with various technical means in the same equipment, and the measuring cavity 500 is provided with:
a fourth interface pair 501 for interfacing with the third interface pair 406;
a fifth sample transfer lever 505 for preparing the nano-materials to be transferred between the measurement chamber 500 and the sample preparation device 40;
a helium tri-refrigerator 507 for refrigerating the measurement cavity 500 and maintaining a very low temperature environment;
a superconducting magnet 509 for generating a magnetic field without energy loss in operation under direct current conditions;
a cold shield 510 for reducing heat radiation leakage from the measuring head 511;
the helium three-refrigeration machine 507 is provided with a liquid nitrogen refrigeration area, a helium four-refrigeration area and a helium three-refrigeration area, a cold screen 510 is installed in the liquid nitrogen refrigeration area and the helium four-refrigeration area, a superconducting magnet 509 is installed in the helium four-refrigeration area and has the structural characteristic that the inner hollow side surface is provided with a hole, and a measuring head 511 is installed in the helium three-refrigeration area to ensure the representation of the nano material in the ultrahigh vacuum extremely low temperature environment;
a third microscopic observation assembly 508 for optically interacting with the measuring head 511 through the cold shield 510 and the superconducting magnet 509, wherein the third microscopic observation assembly 508 may be a long-focus microscope;
in this embodiment, a second observation window 506 for observing the transmission state of the sample is disposed on the measurement cavity 500, so that the transmission state can be conveniently observed during the transmission of the sample;
the measurement cavity 500 is communicated with a sample transfer cavity 503 through a sample transfer assembly 502, the sample transfer cavity 503 is provided with a fifth pair of interfaces 531 communicated with the interconnection channel 60, and the sample transfer cavity 503 is provided with a fourth sample transfer control rod 504 for realizing mutual transfer of the prepared nano materials between the sample transfer cavity 503 and the interconnection channel 60;
in this embodiment, a sample is loaded from the first quick-opening door 301, and is input into the transmission cavity 401 from the first pair of interfaces 302 and the second pair of interfaces 403 and transferred to the sample stage assembly 402 in the preparation cavity 400 by combining with the third sample transfer control rod 412 through the manipulation of the first sample transfer control rod 303, the sample is prepared and processed in the preparation cavity 400 through the evaporation assembly 407 and the etching assembly 408, the prepared and processed nanomaterial is transferred into the measurement cavity 500 through the third pair of interfaces 406 and the fourth pair of interfaces 501, the helium three refrigerator 507 refrigerates the measurement cavity 500 and maintains a very low temperature environment, and the measurement head 511 represents the nanomaterial in an ultrahigh vacuum low temperature environment;
and the fifth interface 531 on the sample transfer cavity 503 is in butt joint with the interconnection channel 60, so that the compatibility requirement of a large-scale measurement experiment station can be met, and meanwhile, other sample preparation and measurement systems can be in butt joint, so that the test on other samples can be realized according to the requirement, and the requirement of continuing other tests on the samples prepared and represented by the device can also be realized.
Example 2
The difference between this embodiment and embodiment 1 is that, as shown in fig. 6, the first pair of interfaces 302, the second pair of interfaces 403, the third pair of interfaces 406, the fourth pair of interfaces 501, and the fifth pair of interfaces 531 are all provided with flexible bellows for ensuring flexible connection of each device and an ultrahigh vacuum gate valve for selectively opening or closing a channel, so that flexible connection between two sets of devices in butt joint can be ensured while the butt joint and intercommunication function is realized, the channel is selectively opened or closed, and mutual influence between the two sets of devices is reduced.
Other undescribed structures refer to example 1.
In this embodiment, abundant system expansion interfaces, such as the expansion flange port 80 in fig. 9, are reserved on the preparation cavity 400, the transmission cavity 401, the measurement cavity 500, and the sample injection cavity 300, so as to be compatible with the subsequent system upgrade requirements and improve the adaptability.
In the description of the present invention, it should be noted that the terms "first", "second", "third", "fourth" and "fifth" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: those skilled in the art can still make modifications or changes to the embodiments described in the foregoing embodiments, or make equivalent substitutions for some features, within the scope of the disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (7)

1. The utility model provides an ultra-high vacuum utmost point low temperature nano-material preparation and characterization equipment, includes strutting arrangement (20) as the installation base member, characterized by still includes: the electric cabinet (10) is used for integrated control of electric elements in the equipment; an interconnected channel (60) for equipment integration to the workstation for transporting the prepared nanomaterial to the next process for in situ measurement;
the top end of the supporting device (20) is provided with a rapid sampling device (30), a sample preparation device (40) and a sample measuring device (50) which are connected in sequence:
quick sampling device (30) for easy-to-wear accessory in quick replacement sample and the equipment under the ultrahigh vacuum state, quick sampling device (30) including set up in advance kind cavity (300) of strutting arrangement (20) upper end, and advance to be equipped with on kind cavity (300):
a first quick-open door (301) for feeding samples and consumable accessories in the apparatus;
a first pair of interfaces (302) for interfacing with a sample preparation device (40);
a first sample transfer control rod (303) for realizing mutual transfer of the sample and consumable fittings in the device between the sample feeding cavity (300) and the sample preparation device (40);
sample preparation device (40) for nanomaterial's preparation and transport under the ultrahigh vacuum state prepares nanomaterial to sample measuring device (50), and sample preparation device (40) is equipped with second to interface (403) with first to interface (302) butt joint on transmission cavity (401) including setting up preparation cavity (400) and the transmission cavity (401) that communicates on preparation cavity (400) in strutting arrangement (20) upper end, preparation cavity (400) on are equipped with:
a third docking interface (406) for docking with a sample measurement device (50);
a sample stage assembly (402) for sample fixation and angle control in an ultra-high vacuum state;
an evaporation component (407) and an etching component (408) for preparing the nano materials with different shapes;
a first microscopic observation assembly (409) for observing the sample stage assembly (40) from directly below;
a second microscopic observation assembly (410) for observing the sample stage assembly (40) from directly in front;
a third sample transfer control rod (412) for realizing mutual transfer of the sample and consumable fittings in the equipment between the rapid sample introduction device (30) and the transmission cavity (401);
a second sample transfer lever (411) for transferring the prepared nanomaterial between the preparation chamber (400) and the sample measuring device (50);
sample measuring device (50) for the nano-material's under the extreme low temperature environment of super high vacuum characterization and transport nano-material to interconnect passageway (60), sample measuring device (50) is including setting up in measurement cavity (500) of strutting arrangement (20) upper end, it has measuring head (511) to the nano-material characterization to measure cavity (500) built-in, is equipped with on measurement cavity (500):
a fourth pair of interfaces (501) for interfacing with the third pair of interfaces (406);
a fifth sample transfer lever (505) for preparing the nanomaterial transferred to and from the measurement chamber (500) and the sample preparation device (40);
a helium tri-refrigerator (507) for refrigerating the measurement cavity (500) and maintaining a very low temperature environment;
a superconducting magnet (509) for generating a magnetic field without energy loss for operation under direct current conditions;
a cold shield (510) for reducing heat radiation leakage from the measuring head (511);
and a third microscopic observation assembly (508) which is used for transmitting the cold shield (510) and the superconducting magnet (509) and performing optical interaction with the measuring head (511).
2. The ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device of claim 1, wherein: the supporting device (20) comprises a supporting frame (201) and a panel (202) arranged on the supporting frame, and the supporting frame (201) is composed of an aluminum section frame and a stainless steel supporting column.
3. The ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device of claim 1, wherein: the preparation cavity (400) and the transmission cavity (401) are respectively provided with a plurality of first observation windows (405) for observing the transmission state of the sample.
4. The ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device of claim 1, wherein: the sample stage assembly (402) comprises:
a sample pedestal (422) for sample fixation and angle control with nanometer precision;
a mask plate seat (423) used for the nanometer material preparation mask plate fixation and the nanometer precision angle control;
the wide-range moving piece (421) is used for realizing the XYZ-axis and rotation four-dimensional movement of the sample pedestal (422) and the mask plate pedestal (423).
5. The ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device of claim 1, wherein: the first pair of interfaces (302), the second pair of interfaces (403), the third pair of interfaces (406), the fourth pair of interfaces (501) and the fifth pair of interfaces (531) are respectively provided with a flexible corrugated pipe for ensuring flexible connection of all devices and an ultrahigh vacuum gate valve for selectively opening or closing a channel.
6. The ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device of claim 1, wherein: the measurement cavity (500) is communicated with a sample transfer cavity (503) through a sample transfer component (502), a fifth butt joint (531) communicated with the interconnection channel (60) is arranged on the sample transfer cavity (503), and a fourth sample transfer control rod (504) used for preparing the nano material and mutually transferring the nano material between the sample transfer cavity (503) and the interconnection channel (60) is arranged on the sample transfer cavity (503).
7. The ultra-high vacuum ultra-low temperature nanomaterial preparation and characterization device of claim 1, wherein: the rapid sampling device (30), the sample preparation device (40) and the sample measurement device (50) are all provided with an ultrahigh vacuum obtaining and measuring assembly (70), and the ultrahigh vacuum obtaining and measuring assembly (70) comprises a vacuum pump set (701) for vacuumizing the interior of the cavity to obtain an ultrahigh vacuum state, a vacuum plate valve (702) for closing an upper opening of the cavity to maintain the ultrahigh vacuum state of the interior of the cavity, and a vacuum gauge (703) for detecting the ultrahigh vacuum state of the interior of the cavity.
CN202210396230.9A 2022-04-15 2022-04-15 Ultrahigh vacuum extremely-low temperature nano material preparation and characterization equipment Active CN114813735B (en)

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CN110487609A (en) * 2019-09-06 2019-11-22 仪晟科学仪器(嘉兴)有限公司 Ultrahigh vacuum in-situ film etches electrode growth system
CN110672453A (en) * 2019-09-10 2020-01-10 中国科学院上海技术物理研究所 Integrated in-situ characterization method for nano material
CN112048704A (en) * 2020-08-13 2020-12-08 北京航空航天大学合肥创新研究院 Integrated processing equipment for ultrathin multilayer film and application method
CN114057159A (en) * 2021-11-18 2022-02-18 仪晟科学仪器(嘉兴)有限公司 Ultrahigh vacuum two-dimensional material preparation system and preparation method

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CN108660419A (en) * 2017-03-31 2018-10-16 中国科学院大连化学物理研究所 One kind is based on volatile corrosion substance film deposition under UHV condition and catalysis reaction test device
CN107525846A (en) * 2017-10-11 2017-12-29 北京大学 A kind of compatible low temperature high-intensity magnetic field original position feeding device of ultrahigh vacuum
CN208432627U (en) * 2018-07-17 2019-01-25 苏州华杨赛斯真空设备有限公司 Portable ultrahigh vacuum sample transfer device
CN110487609A (en) * 2019-09-06 2019-11-22 仪晟科学仪器(嘉兴)有限公司 Ultrahigh vacuum in-situ film etches electrode growth system
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