CN115083872A - Vacuum prestoring device for sample rod of transmission electron microscope - Google Patents
Vacuum prestoring device for sample rod of transmission electron microscope Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
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Abstract
The application relates to a vacuum pre-storage device for a transmission electron microscope sample rod, wherein a vacuum storage chamber is hermetically connected with the transmission sample rod through a transmission sample rod adapter flange; the high vacuum cavity is hermetically connected with a vacuum pump set; the high-vacuum gas path adapter is hermetically connected with the high-vacuum chamber through a high-vacuum gas path angle valve; the vacuum adaptor is hermetically connected with the high-vacuum gas circuit adaptor through a vacuum pipeline. When the transmission sample rod is not used or temporarily stored, the transmission sample rod is stored in a transmission electron microscope sample rod vacuum pre-storage device, and when the transmission sample rod needs to be used, the transmission sample rod is taken out of the transmission electron microscope sample rod vacuum pre-storage device and inserted into a corresponding position of a transmission electron microscope; the vacuum pumping device is favorable for guaranteeing the maximum isolation of the transmission sample rod of the transmission electron microscope from water vapor and pollutants in the atmosphere, greatly shortens the vacuum pumping time of the electron microscope sample, provides a high-vacuum heating degassing design for the freezing transmission sample rod, and simultaneously realizes the high-vacuum heating degassing function of the freezing electron microscope sample rod and the daily vacuum storage function of the conventional sample rod.
Description
Technical Field
The application relates to the field of electron microscope equipment, in particular to vacuum pre-storage equipment for a transmission electron microscope sample rod.
Background
For the conventional Transmission sample rod vacuum storage of a conventional Electron Microscope, i.e. a Transmission Electron Microscope (TEM), the Transmission Electron Microscope sample and the Transmission Electron Microscope sample rod are exposed to the atmosphere for a long time, and moisture and residual pollutants in the air are attached to the surface of the sample/sample rod. When a sample or a sample rod enters a transmission electron microscope, residual water vapor on the surface of the sample or the sample rod comprising the inner surface and the outer surface of the rod is slowly released, so that the vacuum-pumping time of the electron microscope is greatly prolonged, and particularly, the in-situ transmission electron microscope sample rod has a complex internal structure and greatly increased internal surface area, and the phenomenon of vacuum-pumping delay after entering the transmission electron microscope is particularly serious; and the residual pollutants can pollute the sample to be observed, and even can pollute the vacuum chamber of the electron microscope, the inner pole shoe, the detector and other related parts.
For the two problems, the traditional solution is to heat the sample or the sample rod to more than 100 ℃ by adopting a heating table or a halogen lamp and other modes, so that residual water vapor and pollutants are volatilized as much as possible; meanwhile, the sample rod and the sample are stored in a drying box containing a drying agent so as to isolate water vapor and pollutants in the atmosphere.
However, the method of using a drying oven for storage and removing moisture and contaminants by heating still has a great risk, which specifically includes: the drying agent needs to be frequently replaced, water vapor and pollutants in the drying oven cannot be completely isolated from the atmosphere, the sample can be modified in the baking process, the baking time is prolonged from another aspect, and the like.
In addition, for vacuum storage and water vapor removal of the frozen transmission sample rod, the traditional method is to partially fill liquid nitrogen into the dewar tank of the frozen transmission sample rod, and conduct low-temperature heat of the liquid nitrogen to the sample at the end of the sample rod through the internal device of the sample rod, so as to ensure that the sample needs to be transferred, stored or observed at low temperature to maintain a frozen low-temperature state. In order to ensure the isolation of low-temperature liquid nitrogen in the Dewar flask or reduce the heat exchange effect with the outside room temperature atmosphere, the Dewar flask is designed into a double-layer structure, and the middle interlayer is a vacuum heat insulation layer which is similar to a vacuum thermos flask structure. Besides maintaining a certain vacuum degree, the vacuum heat insulating layer of the dewar tank is internally provided with a low-temperature adsorption molecular sieve to adsorb trace water vapor so as to prevent the heat transfer effect of heat conduction and heat convection.
Meanwhile, after the frozen transmission sample rod is used and is drawn out from the transmission electron microscope sample table each time, the exposed part of the sample rod exposed to the atmosphere is usually not higher than-196 ℃ due to the low temperature of liquid nitrogen, and a large amount of water vapor and other gases in the air can be instantly condensed and adsorbed to frost on the surface of the sample rod. Therefore, in order to ensure that the frozen transmission sample rod is quickly recovered after being used, the sample rod and the Dewar flask vacuum interlayer molecular sieve are required to be subjected to vacuum heating degassing regeneration treatment. Namely, the two parts of the frozen transmission sample rod and the vacuum interlayer of the Dewar flask are required to be respectively vacuumized and degassed, and the sample rod is provided with a heating temperature control power supply to realize heating operation. After the freezing transmission sample rod is subjected to vacuum heating degassing regeneration, the vacuum storage state needs to be maintained continuously to isolate water vapor and pollutants in the atmosphere.
However, the mainstream vacuum storage station in the field of the traditional electron microscope cannot simultaneously meet the differentiation requirements of vacuum storage of two transmission sample rods. Meanwhile, the design structure of the existing vacuum storage station is that a plurality of sample rod vacuum chambers are connected in series, so that the vacuum pumping/discharging operation of a single sample rod cannot be independently controlled, and the vacuum storage of other sample rods is not influenced.
Disclosure of Invention
Based on this, it is necessary to provide a vacuum pre-storage device for a sample rod of a transmission electron microscope.
In one embodiment, the vacuum prestore device for the transmission electron microscope sample rod comprises:
the vacuum storage chamber is hermetically connected with the transmission sample rod through a transmission sample rod adapter flange;
an electromagnetic valve;
the vacuum pump sets are hermetically connected with the vacuum storage chambers in a one-to-one correspondence mode through the electromagnetic valves;
the high vacuum chamber is hermetically connected with the vacuum pump set;
a high vacuum gas circuit angle valve;
the high-vacuum gas path adapter is hermetically connected with the high-vacuum chamber through the high-vacuum gas path angle valve;
and the vacuum adaptor is connected with the high-vacuum air path adaptor in a sealing manner through a vacuum pipeline.
When the device is not used or temporarily stored, the transmission sample rod is stored in the vacuum pre-storage equipment of the transmission electron microscope sample rod, when the device is required to be used, the transmission sample rod is taken out of the vacuum pre-storage equipment of the transmission electron microscope sample rod and is inserted into a corresponding position of a transmission electron microscope, and the vacuum degree of each vacuum storage chamber is independently controlled through each electromagnetic valve, so that the vacuum storage chambers can independently work and do not interfere with each other; therefore, the transmission sample rod of the transmission electron microscope is favorably ensured to be isolated from water vapor and pollutants in the atmosphere to the greatest extent, so that the vacuumizing time of the electron microscope sample is favorably shortened, a high-vacuum heating degassing design is provided for the freezing transmission sample rod, the high-vacuum heating degassing function of the freezing electron microscope sample rod and the daily vacuum storage function of the conventional sample rod can be realized simultaneously, the pollution to the vacuum chamber and related parts of the electron microscope is favorably reduced, and the service life of the electron microscope system is ensured.
In one embodiment, the vacuum prestore device for the transmission electron microscope sample rod further comprises a control system, and the control system is respectively connected with the vacuum pump set, the high-vacuum gas circuit angle valve and each electromagnetic valve.
In one embodiment, the vacuum pre-storage device for the transmission electron microscope sample rod further comprises a machine frame assembly, the vacuum storage chamber, the high vacuum chamber and the control system are arranged on the machine frame assembly, and the electromagnetic valve and the vacuum pump set are fixed inside the machine frame assembly; and/or the presence of a catalyst in the reaction mixture,
the control system is a touch system; and/or the presence of a catalyst in the reaction mixture,
the vacuum prestore device for the transmission electron microscope sample rod further comprises a full-range vacuum gauge in sealing connection with the vacuum pump set, and the full-range vacuum gauge is used for detecting and providing the system vacuum degree of the vacuum pump set in real time.
Further, in one embodiment, the control system is further connected to the full-range vacuum gauge, and is configured to control the vacuum pump set to stop and maintain pressure when the system vacuum degree reaches a lower system set vacuum pressure limit, and control the vacuum pump set to automatically start until the system vacuum degree reaches an upper system set vacuum pressure limit when the system vacuum degree reaches an upper set vacuum pressure limit.
In one embodiment, the full-scale vacuum gauge is fixed inside the machine frame assembly; and/or the presence of a catalyst in the reaction mixture,
the high vacuum chamber is aligned with each of the vacuum storage chambers; and/or the presence of a catalyst in the reaction mixture,
the vacuum storage chamber is arranged on the top of the machine frame assembly; and/or the like, and/or,
the control system is arranged on the top or the side part of the machine frame component; and/or the presence of a catalyst in the reaction mixture,
the control switch of the high vacuum chamber is disposed on top of the high vacuum chamber.
In one embodiment, the vacuum prestore device for the transmission electron microscope sample rod further comprises a power supply assembly, and the power supply assembly is respectively connected with the control system, the vacuum pump set, the high-vacuum air path angle valve and each electromagnetic valve.
In one embodiment, the vacuum pre-storage device for the transmission electron microscope sample rod further comprises a machine frame assembly, the vacuum storage chamber, the high vacuum chamber and the control system are arranged on the machine frame assembly, the power supply assembly, the electromagnetic valve and the vacuum pump set are fixed inside the machine frame assembly, and a power switch of the power supply assembly is exposed outside the machine frame assembly; and/or the presence of a catalyst in the reaction mixture,
the control system is a touch system; and/or the presence of a catalyst in the reaction mixture,
the vacuum prestore device for the transmission electron microscope sample rod further comprises a full-range vacuum gauge in sealing connection with the vacuum pump set, and the full-range vacuum gauge is used for detecting and providing the system vacuum degree of the vacuum pump set in real time.
In one embodiment, the vacuum prestoring device for the transmission electron microscope sample rod further comprises the transmission sample rod, wherein the transmission sample rod comprises a conventional transmission sample rod and a frozen transmission sample rod; and/or the presence of a catalyst in the reaction mixture,
the vacuum pre-storage equipment for the transmission electron microscope sample rod further comprises a vacuum tube plug, and the vacuum storage chamber is connected with the transmission sample rod or the vacuum tube plug in a sealing mode through the transmission sample rod adapter flange.
In one embodiment, the vacuum prestorage device for the transmission electron microscope sample rod further comprises transparent glass tubes, and each vacuum storage chamber is connected with one transparent glass tube and one transmission sample rod adapter flange respectively.
In one embodiment, the vacuum prestorage device for the transmission electron microscope sample rod further comprises an infrared lamp, wherein a hot end of the infrared lamp is arranged towards the transparent glass tube and used for baking the transparent glass tube to heat the transmission sample rod therein.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments or the conventional technologies of the present application, the drawings used in the descriptions of the embodiments or the conventional technologies will be briefly introduced below, it is obvious that the drawings in the following descriptions are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an embodiment of a vacuum pre-storage device for a sample rod of a transmission electron microscope according to the present application.
Fig. 2 is another schematic view of the embodiment shown in fig. 1.
Fig. 3 is a schematic perspective view of the embodiment of fig. 1 from another direction.
Fig. 4 is a schematic perspective view of the embodiment of fig. 3 in another direction.
Fig. 5 is a schematic view of the embodiment shown in fig. 4 at a.
FIG. 6 is a schematic diagram illustrating an application of another embodiment of a vacuum pre-storage device for a TEM sample bar according to the present application.
FIG. 7 is a schematic diagram illustrating an application of another embodiment of a vacuum pre-storage device for a TEM sample bar according to the present application.
Reference numerals:
the system comprises a rack assembly 100, a control system 200, a transmission sample rod 310, a vacuum tube plug 320, a transparent glass tube 340, a high vacuum gas path angle valve 350, a high vacuum gas path adapter 360, a high vacuum chamber 370, a transmission sample rod adapter flange 380, a vacuum adapter 390, a vacuum storage chamber 400, a power supply assembly 500, an electromagnetic valve 600, a vacuum pump set 700 and a full-range vacuum gauge 800;
a conventional transmission sample rod 311, a frozen transmission sample rod 312, a control switch 371, a vacuum line 391, and a power switch 510.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present application more comprehensible, embodiments accompanying figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. This application is capable of embodiments in many different forms than those described herein and that modifications may be made by one skilled in the art without departing from the spirit and scope of the application and it is therefore not intended to be limited to the specific embodiments disclosed below.
It will be understood that when an element is referred to as being "secured to" or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used in the description of the present application are for illustrative purposes only and do not represent the only embodiments.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present application, "plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise.
In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may mean that the first feature is in direct contact with the second feature or that the first feature is in indirect contact with the second feature via an intermediate medium. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the description of the present application, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The application discloses a vacuum pre-storage device for a transmission electron microscope sample rod, which comprises a partial structure or a whole structure of the following embodiments; namely, the vacuum prestoring device for the transmission electron microscope sample rod comprises the following partial technical characteristics or all technical characteristics. In an embodiment of the present application, a vacuum pre-storage device for a sample rod of a transmission electron microscope includes: the vacuum storage chamber is hermetically connected with the transmission sample rod through a transmission sample rod adapter flange; an electromagnetic valve; the vacuum pump sets are hermetically connected with the vacuum storage chambers in a one-to-one correspondence mode through the electromagnetic valves; the high vacuum chamber is hermetically connected with the vacuum pump set; a high vacuum gas circuit angle valve; the high-vacuum gas path adapter is connected with the high-vacuum chamber in a sealing way through the high-vacuum gas path angle valve; and the vacuum adapter is connected with the high-vacuum gas path adapter in a sealing manner through a vacuum pipeline. When the device is not used or temporarily stored, the transmission sample rod is stored in the vacuum pre-storage equipment of the transmission electron microscope sample rod, when the device is required to be used, the transmission sample rod is taken out of the vacuum pre-storage equipment of the transmission electron microscope sample rod and is inserted into a corresponding position of a transmission electron microscope, and the vacuum degree of each vacuum storage chamber is independently controlled through each electromagnetic valve, so that the vacuum storage chambers can independently work and do not interfere with each other; therefore, the transmission sample rod of the transmission electron microscope is favorably ensured to be isolated from water vapor and pollutants in the atmosphere to the greatest extent, so that the vacuumizing time of the electron microscope sample is favorably shortened, a high-vacuum heating degassing design is provided for the freezing transmission sample rod, the high-vacuum heating degassing function of the freezing electron microscope sample rod and the daily vacuum storage function of the conventional sample rod can be realized simultaneously, the pollution to the vacuum chamber and related parts of the electron microscope is favorably reduced, and the service life of the electron microscope system is ensured.
The transmission electron microscope sample rod vacuum pre-storage device described in the present application is described in detail below with reference to fig. 1 to 7. In one embodiment, a transmission electron microscope sample rod vacuum pre-storage apparatus is shown in fig. 1 and 2, and includes a transmission sample rod adapter flange 380, a vacuum storage chamber 400, a solenoid valve 600, and a vacuum pump set 700; the vacuum storage chamber 400 is hermetically connected with the transmission sample rod 310 through a transmission sample rod adapter flange 380; the vacuum storage chamber 400 is hermetically connected to the vacuum pump group 700 through the solenoid valve 600; in each embodiment, the connection is sealed to avoid air leakage, thereby ensuring and maintaining the vacuum degree in the corresponding interval. By means of the design, when a sample is not used or temporarily stored, the transmission sample rod with the sample stored therein is stored in the vacuum pre-storage device of the transmission electron microscope sample rod, and when the transmission sample rod with the sample stored therein is required to be used, the transmission sample rod is taken out of the vacuum pre-storage device of the transmission electron microscope sample rod and is inserted into the corresponding position of the transmission electron microscope.
Further, the vacuum storage principle of the conventional transmissive sample rod is explained as follows. The system is provided with an oil-free vacuum environment by using a vacuum pump set 700, such as the vacuum pump set 700 consisting of a turbo molecular pump and an oil-free diaphragm pump. When the transmission sample rod 310 is in an idle state, the sample and the sample rod need to be stored in a vacuum pre-storage device, i.e. a vacuum storage station, of the transmission electron microscope sample rod; when it is desired to use the transmission sample rod 310, the sample and the transmission sample rod 310 are removed from the vacuum storage station and inserted into an electron microscope. So just can guarantee in electron microscope sample and sample rod and the atmosphere steam and pollutant maximum isolated to take away residual gas and pollutant on the sample rod surface, avoid the secondary pollution problem that the sample pretreatment leads to. Meanwhile, the method can effectively ensure that the vacuumizing time of the electron microscope sample is greatly shortened, and reduce the pollution to the vacuum chamber and parts of the electron microscope. In contrast, when a conventional transmission sample rod is exposed to the atmosphere for a long time, water vapor and pollutants in the air can be attached to the surface of the sample rod, and when the polluted sample rod is inserted into an electron microscope, the pollutants on the surface of the sample rod are released, so that the vacuumizing time of the electron microscope is prolonged, and the vacuum chamber, the inner pole shoe, the detector and the like of the electron microscope are further polluted. Such contamination is long term and cumulative, and even with normal maintenance of the electron microscope, can be difficult to remove, which can shorten the life of the electron microscope. This application adopts the scheme that each vacuum storage chamber 400 was controlled respectively to vacuum pump package 700, especially adopts the totally oilless vacuum pump package 700 scheme of turbo molecular pump and diaphragm pump, creates a clean high vacuum environment to transmission electron microscope sample pole, only approximately equals to deposit the steam adsorption capacity of one day in the atmosphere through test transmission sample pole 310 vacuum storage half a year. Consequently, can completely cut off transmission sample pole and atmospheric pollutants through this application, extension transmission electron microscope host computer life, and be favorable to maintaining transmission electron microscope instrument normal operating and stable for a long time.
With reference to fig. 1-7, in one embodiment, the transmission sample rod 310 includes a conventional transmission sample rod 311 and a frozen transmission sample rod 312. The transmission sample rod 310 shown in fig. 1 to 4 is a frozen transmission sample rod 312, the transmission sample rod 310 shown in fig. 6 is a conventional transmission sample rod 311, and the transmission sample rod 310 shown in fig. 7 is a frozen transmission sample rod 312. In order to store the frozen transmission sample rod 312, in one embodiment, the transmission sample rod 310 includes a conventional transmission sample rod 311 and a frozen transmission sample rod 312, and the tem sample rod vacuum pre-storage device further includes a high vacuum gas path angle valve 350, a high vacuum gas path adaptor 360, a high vacuum chamber 370 and a vacuum adaptor 390; the vacuum adaptor 390 is hermetically connected to the high vacuum air path adaptor 360 through a vacuum pipeline 391, the high vacuum air path adaptor 360 is hermetically connected to the high vacuum chamber 370 through the high vacuum air path angle valve 350, and the high vacuum chamber 370 is hermetically connected to the vacuum pump set 700. In various embodiments, the high vacuum chamber 370 has the same or higher vacuum level than the vacuum storage chamber 400, and the vacuum adapter 390 is used for vacuum adapter of the frozen transmission sample rod dewar. Specifically, in one embodiment, a vacuum prestorage device for a transmission electron microscope sample rod is shown in fig. 1 and fig. 2, and includes a high vacuum air path angle valve 350, a high vacuum air path adapter 360, a high vacuum chamber 370, a transmission sample rod adapter flange 380, a vacuum adapter 390, a vacuum pipeline 391, a vacuum storage chamber 400, a solenoid valve 600, and a vacuum pump set 700; the vacuum storage chamber 400 is hermetically connected with the transmission sample rod 310 through a transmission sample rod adapter flange 380; the vacuum storage chamber 400 is hermetically connected to the vacuum pump group 700 through the solenoid valve 600; the high vacuum chamber 370 is sealingly connected to the vacuum pump stack 700; the high-vacuum gas path adapter 360 is hermetically connected with the high-vacuum chamber 370 through the high-vacuum gas path angle valve 350; the vacuum adapter 390 is hermetically connected to the high vacuum air path adapter 360 through the vacuum pipeline 391. The rest of the embodiments are analogized and are not described in detail. In one embodiment, the transmission electron microscope sample rod vacuum pre-storage device further comprises the transmission sample rod 310, and the transmission sample rod 310 comprises a conventional transmission sample rod 311 and a frozen transmission sample rod 312. Such design provides high vacuum heating degasification design to freezing transmission sample pole, has realized freezing transmission sample pole vacuum storage and the moisture demand of removing, is favorable to realizing simultaneously freezing electron microscope sample pole high vacuum heating degasification function and the daily vacuum storage function of conventional sample pole.
Further, considering that the sample rod and the dewar vacuum interlayer of the frozen transmission sample rod 312 require vacuum degassing, in one embodiment, the high vacuum gas path angle valve 350 is linked with each of the solenoid valves 600, and the solenoid valve 600 is used for automatically activating the high vacuum gas path angle valve 350 in a working state, that is, for the frozen transmission sample rod 312, vacuum degassing is simultaneously performed on the sample rod and the dewar vacuum interlayer thereof.
Further, the principle of degassing the transmission sample rod 312, i.e. the cryo-electron microscope sample rod, by high vacuum heating is described as follows. The cryoelectron microscope sample rod needs to remove water vapor and mainly comprises two parts, namely the sample rod and a dewar vacuum interlayer. Removing water vapor from the sample rod by adopting a vacuum storage station of the sample rod of a conventional electron microscope; the dewar vacuum interlayer water vapor removal method is characterized in that a vacuum adapter 390 is connected with a high vacuum gas path adapter 360 through a vacuum pipeline and is vacuum-sealed, and then the vacuum adapter is connected with a high vacuum chamber 370 in a vacuum manner, and the high vacuum gas path angle valve 350 is used for controlling the opening or closing of the vacuum system so as to realize corresponding functions. The design has the high vacuum heating degassing function of the sample rod of the cryo-electron microscope and the daily vacuum storage function of the sample rod of the conventional transmission electron microscope. It can be understood, the heating is based on the traditional method of carrying of getting rid of the steam mode, this application transmission electron microscope sample pole vacuum prestore equipment need not to design heating device and can reach vacuum dewatering promptly vacuum heating degasification function perhaps high vacuum heating degasification function does certainly also to cooperate baking equipment to realize the heating action, and this application has broken through traditional transmission electron microscope sample pole vacuum prestore equipment mainly used and has frozen transmission sample pole vacuum and get rid of steam, has the limitation of conventional transmission sample pole storage function concurrently, adopts compact structure modularized design, and breakthroughly integrated freezing transmission sample pole heating dewaters the steam, freezes transmission sample pole vacuum prestore and the function of conventional transmission sample pole vacuum storage. The vacuum degassing device is particularly suitable for the requirements of high vacuum heating and degassing of the sample rod of the cryoelectron microscope in a laboratory and the requirement of daily vacuum storage of the conventional sample rod. The device can realize the high vacuum heating degassing function of the sample rod of the cryoelectron microscope and the daily vacuum storage function of the conventional sample rod at the same time, and can also realize the application of two functions independently. The functional accessories are not required to be added or reduced, dual-purpose seamless switching use of one machine is realized, and the use efficiency of the equipment is improved.
From a practical point of view, in one embodiment, the number of the vacuum storage chambers 400 is at least two, and the vacuum storage chambers 400 are used for storing a corresponding number of transmission sample rods 310 at the same time, that is, each vacuum storage chamber 400 stores one transmission sample rod 310. Further, in one embodiment, the vacuum storage chambers 400 are spatially formed in a two-layer structure having different heights. Further, in one embodiment, the vacuum storage chambers 400 are arranged in a row, and may be located at the same level or different levels. For embodiments having a high vacuum chamber 370, in one embodiment, the high vacuum chamber 370 is aligned with each of the vacuum storage chambers 400. Further, in one embodiment, the vacuum storage chambers 400 are arranged in a row and located on the same level plane. Further, in one embodiment, the vacuum storage chambers 400 are arranged in two rows and spatially form a two-layer structure having different heights. By the design, multiple storage stations are formed, and the device is compatible with transmission electron microscope sample rods of specified models, such as Thermo, JEOL, HITACHI and the like. The design of this application has many storage stations, can satisfy the demand of many sample poles vacuum prestore simultaneously or timesharing. And every station of this application is compatible at present the sample rod of mainstream transmission electron microscope brand model on the market, plug-and-play, and is safe high-efficient. And on one hand, the multi-path sample rods are switched through independent sample rods, and the vacuum chamber 400 and the electromagnetic valve 600 are connected with the vacuum pump set 700 in parallel, namely, each storage station is vacuumized or vacuumized for independent interlocking operation. Further, the vacuum pumping or vacuum releasing operation of any storage station is realized through the vacuum interlocking of the independent electromagnetic valves 600, and the vacuum storage states of other storage stations are not influenced. On the other hand, the transmission sample rod 310 is beneficial to forming a regular transmission sample rod, is convenient for a user to take and place, and is particularly suitable for being matched with an automatic robot to use.
Further, referring to fig. 2, 4 and 5, the high vacuum chamber 370 and 5 vacuum storage chambers 400 are aligned in a row, and the tem sample rod vacuum pre-storage apparatus is correspondingly provided with 5 electromagnetic valves 600, i.e. 5 tem storage stations are formed, to which 5 tem sample rods 310 can be connected. Because the vacuum storage chamber 400 is hermetically connected with the vacuum pump unit 700 through the electromagnetic valve 600, each storage station is started and stopped independently, and vacuum safety interlocking protection is realized. This application utilizes independent vacuum solenoid valve parallel access vacuum pump package 700 design of each own through each transmission sample pole memory station, realizes that each memory station can independent control evacuation or the operation of putting the vacuum, wherein any memory station evacuation or the operation of putting the vacuum of any way promptly, does not all influence other memory stations vacuum save state, has the interlock protect function of maloperation promptly, guarantees the independent interlocking in vacuum of each transmission electron microscope memory station.
Further, in one embodiment, the vacuum prestorage device for the transmission electron microscope sample rod further includes transparent glass tubes 340, and each of the vacuum prestorage chambers 400 is connected to one of the transparent glass tubes 340 and one of the transmission sample rod adapter flanges 380. Further, in one embodiment, the transmissive sample rod 310 is threaded into the vacuum storage chamber 400 through the transmissive sample rod adapter flange 380 and partially positioned in the transparent glass tube 340. The design is favorable for an operator to observe the end part of the sample rod of the transmission electron microscope and the state of a sample fixed by the end part, and the end part and the sample of the sample rod can be further baked by an infrared lamp so as to realize the purpose of heating and degassing. Further, in one embodiment, the vacuum pre-storage device for the transmission electron microscope sample rod further includes an infrared lamp or is further connected with the infrared lamp, and a hot end of the infrared lamp is disposed toward the transparent glass tube 340 and is used for baking the transparent glass tube 340 to heat the transmission sample rod 310 therein. Further, the transparent glass tube 340 is a quartz glass tube. Further, in one embodiment, for the transparent glass tube 340 and the transmissive sample rod adapter flange 380 connected to the vacuum storage chamber 400, the transparent glass tube 340 and the transmissive sample rod adapter flange 380 are coaxially disposed and respectively located at two sides of the vacuum storage chamber 400. Further, in one embodiment, two transmissive sample rod adaptor flanges 380 are positioned on opposite sides of adjacent two of the vacuum storage chambers 400. By means of the design, the vacuum pre-storage equipment for the transmission electron microscope sample rod is compact in structure and high in use efficiency, can meet the requirements for a high-vacuum heating and degassing function of the freezing electron microscope sample rod and a daily vacuum storage function of a conventional sample rod, can simultaneously realize the high-vacuum heating and degassing function of the freezing electron microscope sample rod and the daily vacuum storage function of the conventional sample rod, and can also respectively and independently realize application of the two functions; need not to add and subtract functional accessories, can realize a dual-purpose seamless switching of a machine and use, solved because the relevant system structure that exists at present is complicated, the commonality is not strong in transmission sample pole vacuum storage commonality that leads to not strong, problem with high costs, be favorable to adapting to the conventional transmission sample pole 311 and the freezing transmission sample pole 312 of different volumes, be favorable to make full use of the space, and reduce the volume of product under the prerequisite of equal transmission sample pole 310 holding capacity.
When the number of transmission sample rods 310 is insufficient, or too many samples are temporarily not needed, or when the transmission sample rods 310 are in an external use state, in one embodiment, the transmission electron microscope sample rod vacuum pre-storage device further includes a vacuum pipe plug 320, and the vacuum storage chamber 400 is hermetically connected to the transmission sample rod 310 or the vacuum pipe plug 320 through the transmission sample rod adapter flange 380. In one embodiment, the tem sample rod vacuum pre-storage device further comprises a vacuum pipe plug 320, and the tem adapter flange 380 is hermetically connected to the tem 310 or the vacuum pipe plug 320, so that the vacuum storage chamber 400 is hermetically connected to the tem 310 or the vacuum pipe plug 320 through the tem adapter flange 380. That is, the vacuum pipe block 320 may be used to block the transmission sample rod adapter flange 380, and at this time, the transmission sample rod adapter flange 380 does not need to be connected to the transmission sample rod 310, and the design of the vacuum pipe block 320 is beneficial to maintain the cleanliness of the vacuum storage chamber 400 and the transmission sample rod adapter flange 380 in a state where the transmission sample rod 310 is not connected, for example, in a state where the transmission sample rod 310 is loaded on a microscope or in a state where the transmission sample rod 310 is not installed, and at this time, the sample may also be stored in the vacuum storage chamber 400.
In one embodiment, the vacuum prestore device for the transmission electron microscope sample rod further comprises a control system 200, and the control system 200 is respectively connected with the vacuum pump set 700, the high-vacuum gas circuit angle valve 350 and each electromagnetic valve 600. In one embodiment, the control system 200 is a touch system. The control system 200 is used for controlling the working states of the vacuum pump group 700, the high-vacuum air path angle valve 350 and each solenoid valve 600. In one embodiment, for the embodiment with the control system 200, the tem sample rod vacuum prestorage device further includes a power supply assembly 500, and the power supply assembly 500 is respectively connected to the control system 200, the vacuum pump assembly 700, the high vacuum gas path angle valve 350 and each of the solenoid valves 600 for supplying power.
In one embodiment, the tem sample rod vacuum pre-storage device further comprises a rack assembly 100, the vacuum storage chamber 400, the high vacuum chamber 370 and the control system 200 are disposed on the rack assembly 100, and the solenoid valve 600 and the vacuum pump set 700 are fixed inside the rack assembly 100; referring to fig. 3 and 4, in one embodiment, the solenoid valve 600, the vacuum pump set 700 and the full-range vacuum gauge 800 are fixed inside the gantry assembly 100; in one embodiment, the vacuum storage chamber 400 is disposed on top of the gantry assembly 100; in one embodiment, for embodiments having a control system 200, the control system 200 is disposed on the top or side of the stand assembly 100. Further, in one embodiment, for embodiments having a high vacuum chamber 370, as shown in FIG. 2, a control switch 371 of the high vacuum chamber 370 is disposed on top of the high vacuum chamber 370. Further, the number of the high-vacuum gas path adapters 360 and the high-vacuum gas path angle valves 350 is two, two of the high-vacuum gas path adapters 360 are symmetrically arranged with respect to the high-vacuum chamber 370, two of the high-vacuum gas path angle valves 350 are also symmetrically arranged with respect to the high-vacuum chamber 370, and one of the high-vacuum chambers 370 is hermetically connected to two of the high-vacuum gas path adapters 360 through two of the high-vacuum gas path angle valves 350, so as to be separately or simultaneously connected to two of the vacuum pipelines 391, and separately or simultaneously connected to two of the vacuum adapters 390 through two of the vacuum pipelines 391, that is, the tem sample rod vacuum prestoring device has a storage capacity of being simultaneously connected to two of the frozen tem sample rods 312. As shown in fig. 2, the tem vacuum pre-storage device has 5 vacuum storage chambers 400, which can simultaneously access 5 tem rods 310 and two tem rods 312; the availability of the high vacuum chamber 370 with respect to the two high vacuum gas path angle valves 350 may also be controlled individually by controlling a switch 371.
In one embodiment, the device for vacuum storage and water vapor removal of the sample rod of the transmission electron microscope belongs to the field of electron microscope devices and can be used as an accessory of an electron microscope; the vacuum prestore equipment for the transmission electron microscope sample rod comprises a rack assembly 100, a control system 200, a transparent glass tube 340, a high-vacuum air path angle valve 350, a high-vacuum air path adapter 360, a high-vacuum chamber 370, a transmission sample rod adapter flange 380, a vacuum adapter 390, a vacuum storage chamber 400, a power supply assembly 500, an electromagnetic valve 600, a vacuum pump set 700 and the like. The vacuum degassing device has the high-vacuum heating degassing function of the sample rod of the cryo-electron microscope and the daily vacuum storage function of the sample rod of the conventional transmission electron microscope, ensures vacuum degassing of the sample rod of the cryo-electron microscope and the Dewar flask, and has zero noise and zero vibration during vacuum storage of the sample rod of the conventional transmission electron microscope; the embodiment also has the function of vacuum automatic pressure maintaining, and can independently control each vacuum storage station.
In one embodiment, the vacuum prestore device for the transmission electron microscope sample rod further includes a power supply assembly 500, and the power supply assembly 500 is respectively connected to the control system 200, the vacuum pump assembly 700, the high-vacuum air path angle valve 350, and each of the electromagnetic valves 600. In one embodiment, the tem sample rod vacuum pre-storage apparatus further comprises a rack assembly 100, the vacuum storage chamber 400, the high vacuum chamber 370 and the control system 200 are disposed on the rack assembly 100, the power supply assembly 500, the solenoid valve 600 and the vacuum pump assembly 700 are fixed inside the rack assembly 100, and the power switch 510 of the power supply assembly 500 is exposed outside the rack assembly 100. In one embodiment, the vacuum prestorage device for the transmission electron microscope sample rod comprises a rack assembly 100, a control system 200, a transparent glass tube 340, a high-vacuum air path angle valve 350, a high-vacuum air path adapter 360, a high-vacuum chamber 370, a transmission sample rod adapter flange 380, a vacuum adapter 390, a vacuum storage chamber 400, a power supply assembly 500, a solenoid valve 600 and a vacuum pump set 700; the transparent glass tube 340 and the transmission sample rod adapter flange 380 are connected to the vacuum storage chamber 400 in a vacuum sealing manner; a conventional transmission sample rod or frozen transmission sample rod or vacuum tube block 320 is connected and vacuum sealed in the vacuum storage chamber 400 by a transmission sample rod adaptor flange 380; the vacuum pre-storage device for the transmission electron microscope sample rod is provided with x sets of vacuum storage chambers 400, namely x conventional transmission sample rods or freezing transmission sample rods or vacuum tube plugs 320 are connected and vacuum-sealed in the x sets of vacuum storage chambers 400 through x transmission sample rod adapter flanges 380; x is an integer of 1 or more. In one embodiment, y high vacuum gas path adapters 360 are connected in the high vacuum chamber 370 through y high vacuum gas path angle valves 350; the vacuum adaptor 390 is connected and vacuum sealed on the high vacuum gas path adaptor 360 through a vacuum pipeline, and further vacuum connected in the high vacuum chamber 370; y is an integer, and x is equal to or greater than y and y is equal to or greater than 1. In one embodiment, the x sets of vacuum storage chambers 400 are vacuum connected to the vacuum pump set 700 by x solenoid valves 600; high vacuum chamber 370 is vacuum connected to vacuum pump stack 700; the full-range vacuum gauge 14 is connected to the vacuum pump set 700 in a vacuum manner and displays the vacuum degree of the system in real time; in this embodiment, the vacuum pump unit 700 includes a turbo molecular pump and a diaphragm pump, so as to implement high-vacuum oil-free environment storage and ensure cleanliness of a vacuum system; x is an integer of 1 or more.
In one embodiment, the vacuum pre-storage device for the sample rod of the transmission electron microscope further comprises a full-range vacuum gauge 800 hermetically connected with the vacuum pump unit 700, wherein the full-range vacuum gauge 800 is used for detecting and providing the system vacuum degree of the vacuum pump unit 700 in real time. In one embodiment, for embodiments having a gantry assembly 100, the full-scale vacuum gauge 800 is affixed to the interior of the gantry assembly 100. Further, in one embodiment, for the embodiment having the control system 200, the control system 200 is further connected to the full-range vacuum gauge 800, and is configured to control the vacuum pump set 700 to stop and maintain pressure when the system vacuum degree reaches the system set vacuum pressure lower limit, and control the vacuum pump set 700 to automatically start until the system vacuum degree reaches the system set vacuum pressure lower limit when the system vacuum degree reaches the set vacuum pressure upper limit. In one embodiment, the x-set of vacuum storage chambers 400, high vacuum chamber 370, and control system 200 are secured outside the gantry assembly 100; the x electromagnetic valves 600, the vacuum pump set 700 and the full-range vacuum gauge 14 are fixed in the rack assembly 100; the whole machine equipment is powered by the power supply assembly 500 and is controlled by the control system 200; x is an integer of 1 or more. In the design, each independent transmission sample rod storage station adopts automatic vacuum pressure maintaining setting, namely when the lower limit of the set vacuum pressure of the system is reached, the vacuum pump set 700 stops and maintains pressure; when the system slowly boosts pressure to reach the set upper vacuum pressure limit, the vacuum pump set 700 is automatically started until the system pressure reaches the set lower vacuum pressure limit. The automatic vacuum pressure maintaining design of the system can achieve the purposes of zero noise and zero vibration in the vacuum storage process of the sample rod, and external interference on the operation of the transmission electron microscope is reduced to the maximum extent. Thereby realized the automatic vacuum pressurize of vacuum prestore station and set for to make this application automatic vacuum pressurize design can realize zero noise and zero vibrations purpose among the sample pole vacuum storage process, furthest reduces the external disturbance to the transmission electron microscope host computer operation.
In one embodiment, the transparent glass tube 340 and the transmissive sample rod adaptor flange 380 are vacuum-tightly attached to the vacuum storage chamber 400; the conventional transmission sample rod 311 or the frozen transmission sample rod 312 or the vacuum tube block 320 is connected and vacuum-sealed in the vacuum storage chamber 400 through the transmission sample rod adapter flange 380; the high vacuum gas path adapter 360 is connected into the high vacuum chamber 370 through the high vacuum gas path angle valve 350; the vacuum adaptor 390 is connected and vacuum sealed on the high vacuum gas path adaptor 360 through a vacuum pipeline, and further vacuum connected in the high vacuum chamber 370; the vacuum storage chamber 400 is vacuum connected to the vacuum pump stack 700 by the solenoid valve 600; high vacuum chamber 370 is vacuum connected to vacuum pump stack 700; the full-range vacuum gauge 800 is connected to the vacuum pump set 700 in a vacuum manner and displays the vacuum degree of the system in real time; the vacuum storage chamber 400, the high vacuum chamber 370 and the control system 200 are fixed outside the machine frame assembly 100; the electromagnetic valve 600, the vacuum pump set 700 and the full-range vacuum gauge 800 are fixed inside the rack assembly 100; the whole equipment is powered by the power supply assembly 500 and is controlled by the control system 200.
Further, in one embodiment, the vacuum pre-storage device for the transmission electron microscope sample rod comprises: the rack assembly 100, the control system 200, the transmission sample rod 310, the transparent glass tube 340, the transmission sample rod adapter flange 380, the vacuum storage chamber 400, the power supply assembly 500, the solenoid valve 600 and the vacuum pump set 700; the vacuum storage chamber 400 and the control system 200 are disposed on the rack assembly 100, the power supply assembly 500, the solenoid valve 600 and the vacuum pump assembly 700 are fixed inside the rack assembly 100, the power switch 510 of the power supply assembly 500 is exposed outside the rack assembly 100, and the power supply assembly 500 is connected to the control system 200, the solenoid valve 600 and the vacuum pump assembly 700, respectively; the control system 200 is respectively connected with the vacuum pump set 700, the high-vacuum air path angle valve 350 and each electromagnetic valve 600; the vacuum storage chamber 400 is respectively connected with one transparent glass tube 340 and one transmission sample rod adapter flange 380, and the vacuum storage chamber 400 is hermetically connected with the vacuum pump set 700 through the solenoid valve 600; the transmissive sample rod adaptor flange 380 is sealingly coupled to the transmissive sample rod 310 such that the vacuum storage chamber 400 is sealingly coupled to the transmissive sample rod 310 via the transmissive sample rod adaptor flange 380. The design has high automation degree, one key is started and stopped, and the plug and play function is realized. The vacuum acquisition and the vacuum breaking are controlled by a set of control system 200, the multi-path transmission electron microscope sample rod vacuum pre-storage station is used for air pumping or air discharging operation, the real-time air pressure of the system, the real-time temperature and rotating speed data of the molecular pump are displayed, and the power supply is started and stopped. The mobile is good, integrates the degree height, and area is little, only needs about a desktop printer size for example, can operate after utilizing 220V civilian power switch-on anytime and anywhere.
Further, in one embodiment, the vacuum prestore device for the sample rod of the transmission electron microscope comprises a rack assembly 100, a control system 200, a transmission sample rod 310, a vacuum pipe plug 320, a transparent glass pipe 340, a high-vacuum air path angle valve 350, a high-vacuum air path adapter 360, a high-vacuum chamber 370, a transmission sample rod adapter flange 380, a vacuum adapter 390, a vacuum storage chamber 400, a power supply assembly 500, an electromagnetic valve 600, a vacuum pump set 700 and a full-range vacuum gauge 800; the vacuum storage chamber 400, the high vacuum chamber 370 and the control system 200 are disposed on the machine frame assembly 100, the power supply assembly 500, the solenoid valve 600 and the vacuum pump unit 700 are fixed inside the machine frame assembly 100, the power switch 510 of the power supply assembly 500 is exposed outside the machine frame assembly 100, and the power supply assembly 500 is connected to the control system 200, the solenoid valve 600 and the vacuum pump unit 700, respectively; the control system 200 is respectively connected with the full-range vacuum gauge 800, the vacuum pump unit 700, the high-vacuum gas circuit angle valve 350 and the electromagnetic valves 600, the full-range vacuum gauge 800 is used for detecting and providing the system vacuum degree of the vacuum pump unit 700 in real time, the control system 200 controls the vacuum pump unit 700 to stop and maintain pressure when the system vacuum degree reaches the system set vacuum pressure lower limit, and controls the vacuum pump unit 700 to automatically start until the system vacuum degree reaches the system set vacuum pressure lower limit when the system vacuum degree reaches the set vacuum pressure upper limit; the vacuum storage chamber 400 is respectively connected with one transparent glass tube 340 and one transmission sample rod adapter flange 380, and the vacuum storage chamber 400 is hermetically connected with the vacuum pump set 700 through the solenoid valve 600; the transmission sample rod adapter flange 380 is hermetically connected with the transmission sample rod 310 or the vacuum pipe plug 320, so that the vacuum storage chamber 400 is hermetically connected with the transmission sample rod 310 or the vacuum pipe plug 320 through the transmission sample rod adapter flange 380, and the vacuum pipe plug 320 is used for plugging the transmission sample rod adapter flange 380 to ensure the system vacuum degree or replacing the transmission sample rod 310 with the sample during detection; the vacuum adaptor 390 is hermetically connected to the high vacuum air path adaptor 360 through a vacuum pipeline 391, the high vacuum air path adaptor 360 is hermetically connected to the high vacuum chamber 370 through the high vacuum air path angle valve 350, and the high vacuum chamber 370 is hermetically connected to the vacuum pump set 700.
Further, in one embodiment, the number of the vacuum storage chambers 400 and the number of the solenoid valves 600 are both five, and the number of the high-vacuum air path angle valves 350 and the high-vacuum air path adapters 360 are both two; alternatively, in one embodiment, the number of the vacuum storage chambers 400 and the number of the solenoid valves 600 are three, and the number of the high-vacuum air path angle valve 350 and the high-vacuum air path adapter 360 are one. In one embodiment, x is 5 and y is 2; the 5 conventional transmission sample rods or freezing transmission sample rods or vacuum tube plugs 320 are connected and vacuum sealed in the 5 sets of vacuum storage chambers 400 through the 5 transmission sample rod adapter flanges 380 and are vacuum connected to the vacuum pump set 700 through the 5 solenoid valves 600; the 2 high vacuum air-path adapters 360 are connected in the high vacuum chamber 370 through the 2 high vacuum air-path angle valves 350 and directly connected to the vacuum pump set 700. In one embodiment, x is 3 and y is 1; the 3 conventional transmission sample rods 311 or the frozen transmission sample rods 312 or the vacuum tube plugs 320 are connected and vacuum-sealed in the 3 sets of vacuum storage chambers 400 through the 3 transmission sample rod adapter flanges 380 and are vacuum-connected to the vacuum pump set 700 through the 3 electromagnetic valves 600; the 1 high vacuum air path adapter 360 is connected in the high vacuum chamber 370 through the 1 high vacuum air path angle valve 350 and directly to the vacuum pump set 700. The design breakthroughly adopts the design of double vacuum air pumping paths, realizes the high vacuum heating and degassing functions of the sample rod of the cryo-electron microscope and the daily vacuum storage function of the sample rod of the conventional transmission electron microscope, and forms the vacuum pre-storage equipment for the sample rod of the transmission electron microscope. The vacuum heating degassing requirement of freezing sample pole has been solved to this application, zero noise and zero vibrations demand when also having conventional sample pole vacuum storage concurrently. Meanwhile, a set of parallel air pumping system is creatively designed according to the requirement of independent storage operation of the plurality of paths of transmission electron microscope sample rods, and the vacuum pumping or vacuum releasing operation of each storage station is independently controlled through a touch screen, so that the vacuum automatic pressure maintaining function of each transmission electron microscope sample rod storage station is ingeniously realized.
In one embodiment, as shown in fig. 6, 2 conventional transmission sample rods 311 and 3 vacuum tube plugs 320 are connected via respective transmission sample rod adapter flanges 380 and are independently vacuum-sealed in 5 sets of vacuum storage chambers 400, i.e. 2 conventional transmission sample rods 311 are vacuum-stored in the tem sample rod vacuum prestoring device of the present application. When it is required to take out 1 or 2 of the conventional transmission sample rods stored in vacuum, the corresponding vacuum storage chamber 400 button in the control system 200 is clicked. At this point, the respective vacuum chambers rupture the exhaust gas and remove the stored transmission sample rod 311 while the other stations are still in vacuum. When the transmission sample rod 311 or the vacuum tube plug 320 is inserted into the empty storage station again, the corresponding vacuum storage chamber 400 button in the control system 200 is clicked again, the vacuum pump set 700 is started and performs vacuum pumping operation on the corresponding station until the lower limit of the vacuum pressure set by the system is reached, and the vacuum pump set 700 is stopped and maintained.
Another embodiment is shown in fig. 7, wherein 1 frozen transmission sample rod 312 and 4 vacuum tube plugs 320 are connected via respective transmission sample rod adapter flanges 380 and independently vacuum-sealed in 5 sets of vacuum storage chambers 400, i.e. 1 frozen transmission sample rod 312 is heated, degassed and vacuum-stored in the tem sample rod vacuum prestorage device of the present application. Wherein, the high vacuum air path adapter 360 is connected to the vacuum adapter 390 through a vacuum line in a vacuum sealing manner. High vacuum gas circuit angle valve 350 opens, guarantees that vacuum pump package 700 can provide the high vacuum environment to freezing transmission sample pole's dewar jar, and freezing transmission sample pole dewar jar heating device starts simultaneously, realizes freezing transmission sample pole dewar jar partial vacuum heating degasification function. When the heating degassing operation of the frozen transmission sample rod is finished, the high vacuum gas path angle valve 350 needs to be closed, that is, the vacuum pump set 700 is closed to enable the vacuum pumping operation of the frozen transmission sample rod dewar. At the same time, when it is desired to remove the vacuum stored frozen transmission sample rod, the corresponding vacuum storage chamber 400 button in the control system 200 is clicked. At this point, the respective vacuum chamber vents and removes the stored frozen transmission sample rod while the other stations remain in vacuum. When the storage station is inserted into the frozen transmission sample rod or the vacuum tube block 320 again, the corresponding vacuum storage chamber 400 button in the control system 200 is clicked again, the vacuum pump set 700 is started and performs vacuum pumping operation on the corresponding station until the lower limit of the vacuum pressure set by the system is reached, and the vacuum pump set 700 is stopped and maintained.
It should be noted that other embodiments of the present application further include a vacuum prestoring device for a transmission electron microscope sample rod, which is formed by combining technical features of the foregoing embodiments with each other and can be implemented.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the claims. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, and these are all within the scope of protection of the present application. Therefore, the protection scope of the present application shall be subject to the appended claims.
Claims (10)
1. The utility model provides a transmission electron microscope sample pole vacuum prestore equipment which characterized in that includes:
a vacuum storage chamber (400) hermetically connected with the transmission sample rod (310) through a transmission sample rod adapter flange (380);
a solenoid valve (600);
the vacuum pump groups (700) are hermetically connected with the vacuum storage chambers (400) through the solenoid valves (600) in a one-to-one correspondence manner;
a high vacuum chamber (370) sealingly connected to the vacuum pump stack (700);
a high vacuum gas path angle valve (350);
the high-vacuum gas path adapter (360) is hermetically connected with the high-vacuum chamber (370) through the high-vacuum gas path angle valve (350);
and the vacuum adaptor (390) is connected with the high-vacuum air channel adaptor (360) in a sealing way through a vacuum pipeline (391).
2. The vacuum prestore device of the TEM sample rod as claimed in claim 1, further comprising a control system (200), wherein the control system (200) is respectively connected to the vacuum pump set (700), the high-vacuum gas circuit angle valve (350) and each of the solenoid valves (600).
3. The TEM sample rod vacuum prestore apparatus as claimed in claim 2, further comprising a machine frame assembly (100), wherein the vacuum storage chamber (400), the high vacuum chamber (370) and the control system (200) are disposed on the machine frame assembly (100), and the solenoid valve (600) and the vacuum pump set (700) are fixed inside the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
the control system (200) is a touch system; and/or the presence of a catalyst in the reaction mixture,
the vacuum prestore device for the transmission electron microscope sample rod further comprises a full-range vacuum gauge (800) connected with the vacuum pump set (700) in a sealing mode, and the full-range vacuum gauge (800) is used for detecting and providing the system vacuum degree of the vacuum pump set (700) in real time.
4. The TEM sample rod vacuum prestore device as recited in claim 3, wherein the full-range vacuum gauge (800) is fixed inside the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
the vacuum storage chamber (400) is disposed on top of the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
the control system (200) is arranged on the top or the side part of the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
a control switch (371) of the high vacuum chamber (370) is disposed on top of the high vacuum chamber (370).
5. The TEM sample rod vacuum prestore device as recited in claim 2, further comprising a power supply assembly (500), wherein the power supply assembly (500) is respectively connected to the control system (200), the vacuum pump set (700), the high vacuum gas path angle valve (350) and each solenoid valve (600).
6. The TEM sample rod vacuum prestore apparatus as claimed in claim 5, further comprising a machine frame assembly (100), wherein the vacuum storage chamber (400), the high vacuum chamber (370) and the control system (200) are disposed on the machine frame assembly (100), the power supply assembly (500), the solenoid valve (600) and the vacuum pump set (700) are fixed inside the machine frame assembly (100), and the power switch (510) of the power supply assembly (500) is exposed outside the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
the control system (200) is a touch system; and/or the presence of a catalyst in the reaction mixture,
the vacuum prestore device for the transmission electron microscope sample rod further comprises a full-range vacuum gauge (800) connected with the vacuum pump set (700) in a sealing mode, and the full-range vacuum gauge (800) is used for detecting and providing the system vacuum degree of the vacuum pump set (700) in real time.
7. The TEM sample rod vacuum prestore device as recited in claim 6, wherein the full-range vacuum gauge (800) is fixed inside the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
the high vacuum chamber (370) is aligned with each of the vacuum storage chambers (400); and/or the presence of a catalyst in the reaction mixture,
the vacuum storage chamber (400) is disposed on top of the machine frame assembly (100); and/or the presence of a catalyst in the reaction mixture,
the control system (200) is arranged on the top or the side part of the machine frame assembly (100); and/or the like, and/or,
a control switch (371) of the high vacuum chamber (370) is disposed on top of the high vacuum chamber (370).
8. The TEM sample rod vacuum prestore apparatus as claimed in claim 1, further comprising the transmission sample rod (310), wherein the transmission sample rod (310) comprises a conventional transmission sample rod (311) and a frozen transmission sample rod (312); and/or the presence of a catalyst in the reaction mixture,
the vacuum prestorage device for the transmission electron microscope sample rod further comprises a vacuum tube plug (320), and the vacuum storage chamber (400) is connected with the transmission sample rod (310) or the vacuum tube plug (320) in a sealing mode through the transmission sample rod adapter flange (380).
9. The TEM sample rod vacuum prestorage device as claimed in any one of claims 1 to 8, further comprising transparent glass tubes (340), wherein each vacuum prestorage chamber (400) is connected to one transparent glass tube (340) and one transmission sample rod adapter flange (380).
10. The TEM sample rod vacuum prestore device as recited in claim 9, further comprising an infrared lamp, wherein a hot end of the infrared lamp is disposed towards the transparent glass tube (340), and is used for baking the transparent glass tube (340) to heat the transmission sample rod (310) therein.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210790496.1A CN115083872A (en) | 2022-07-06 | 2022-07-06 | Vacuum prestoring device for sample rod of transmission electron microscope |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210790496.1A CN115083872A (en) | 2022-07-06 | 2022-07-06 | Vacuum prestoring device for sample rod of transmission electron microscope |
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| CN115083872A true CN115083872A (en) | 2022-09-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210790496.1A Pending CN115083872A (en) | 2022-07-06 | 2022-07-06 | Vacuum prestoring device for sample rod of transmission electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115083872A (en) |
-
2022
- 2022-07-06 CN CN202210790496.1A patent/CN115083872A/en active Pending
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