A sealed and vacuum transfer device of sample for cross platform is connected
阅读说明:本技术 一种用于跨平台连接的样品密封和真空转移装置 (A sealed and vacuum transfer device of sample for cross platform is connected ) 是由 谭军 唐培� 李峰 于 2019-10-14 设计创作,主要内容包括:本发明涉及材料测试技术领域,具体为一种用于电镜或微纳激光加工系统跨平台连接的样品密封和真空转移装置。该装置包括:用于连接电镜真空样品室或者激光加工系统真空腔体侧壁的矩形气密法兰、用于封装测试样品的真空密封转移盒,用于实现样品与电镜或者微纳激光加工系统衔接的高精度支架和夹具结构、用于控制真空密封转移盒的机械臂解锁机构,用于真空密封转移盒安放和更换的真空过渡仓,用于确定真空密封转移盒的开启状态的观察窗,用于观察开启的仓门。本发明可以广泛应用于各种型号扫描电镜、电子束及离子束双束电镜或微纳激光加工系统跨平台连接和真空转移,形成系统性样品装配、保护、转移和送入装置。(The invention relates to the technical field of material testing, in particular to a sample sealing and vacuum transfer device for cross-platform connection of an electron microscope or micro-nano laser processing system. The device includes: the device comprises a rectangular airtight flange used for connecting the side wall of a vacuum sample chamber of an electron microscope or a vacuum cavity of a laser processing system, a vacuum seal transfer box used for packaging a test sample, a high-precision support and clamp structure used for realizing the connection of the sample and the electron microscope or the micro-nano laser processing system, a mechanical arm unlocking mechanism used for controlling the vacuum seal transfer box, a vacuum transition bin used for placing and replacing the vacuum seal transfer box, an observation window used for determining the opening state of the vacuum seal transfer box and a bin gate used for observing the opening state. The invention can be widely applied to cross-platform connection and vacuum transfer of various types of scanning electron microscopes, electron beam and ion beam double-beam electron microscopes or micro-nano laser processing systems to form a systematic sample assembling, protecting, transferring and feeding device.)
1. A sample sealing and vacuum transfer device for cross-platform connection, comprising: the device comprises a rectangular airtight flange, a vacuum transition bin, a bin door, a sample transfer rod vacuum pipeline, a sample transfer rod external controller, a manual rotating unlocking valve, a magnetic coupling sample transfer rod, a vacuum seal transfer box, a sample transfer rod clamp and an observation window, wherein the rectangular airtight flange is used for connecting a vacuum sample chamber and the vacuum transition bin of an electron microscope or a micro-nano laser processing system, the vacuum transition bin is used for placing and replacing a vacuum seal transfer box, the bin door is used for observing opening, the sample transfer rod vacuum pipeline, the sample transfer rod external controller, the manual rotating unlocking valve is used for magnetically coupling the sample transfer rod, the vacuum:
the vacuum transition bin is of a five-channel structure with a front channel, a rear channel, a left channel, a right channel and an upper channel, and a flange is arranged at the port of each channel; the port parts of the front channel and the rear channel of the vacuum transition bin are respectively provided with a bin door and an observation window, the bin door is hermetically connected with the front channel of the vacuum transition bin through a flange, and the observation window is hermetically connected with the rear channel of the vacuum transition bin through a flange; a flange at the port of a left channel of the vacuum transition bin is a rectangular airtight flange; a sample transfer rod vacuum pipeline is arranged at the right channel port of the vacuum transition bin and is hermetically connected with the right channel of the vacuum transition bin through a flange; a rotary unlocking manual valve is installed at the port of an upper channel of the vacuum transition bin, and the rotary unlocking manual valve is hermetically connected with the upper channel of the vacuum transition bin through a flange;
one end of the magnetic coupling sample transfer rod penetrates through the left channel and the right channel of the vacuum transition bin, is matched with a slide way in the sample transfer rod vacuum pipeline and slides in the sample transfer rod vacuum pipeline in a reciprocating manner; the sample transfer rod external controller is arranged on the sample transfer rod vacuum pipeline, the magnetic coupling sample transfer rod and the sample transfer rod external controller realize non-contact connection in a magnetic coupling mode, and the magnetic coupling sample transfer rod realizes displacement control through the sample transfer rod external controller; the other end of the magnetic coupling sample transfer rod is provided with a sample transfer rod clamp, and the vacuum sealing transfer box is arranged on the sample transfer rod clamp.
2. The device for sealing and transferring samples connected across a platform according to claim 1, wherein a left channel of the vacuum transition bin is connected with a side wall of a vacuum sample chamber of an electron microscope or a micro-nano laser processing system through a matched vacuum rubber ring and a rectangular airtight flange, and a right channel of the vacuum transition bin is connected with a matched sample transfer rod vacuum pipeline and a matched sample transfer rod external controller.
3. The device for sealing and transferring samples connected across a platform according to claim 1, wherein the rectangular airtight flange is a variable cross-section flange, one side of which is connected with the side wall of the vacuum sample chamber of the electron microscope or the micro-nano laser processing system and has a relatively large area, and the other side of which is communicated with the side wall of the vacuum transition bin and has a relatively small diameter for adapting to the size and ensuring the sealing performance.
4. The apparatus of claim 1, wherein the vacuum transition chamber has an openable chamber door that is closed and locked to the vacuum transition chamber by a vacuum clamp.
5. The apparatus for sample sealing and vacuum transfer for cross-platform connection according to claim 1, wherein the sample transfer rod fixture fixes the relative position of the vacuum seal transfer box during the moving process and the opening process of the vacuum seal transfer box top cover, the vacuum seal transfer box enters the vacuum transition bin under the driving of the magnetic coupling sample transfer rod, and the vacuum seal transfer box is installed and taken out after the bin door of the vacuum transition bin is opened; the vacuum sealing transfer box is connected with the magnetic coupling sample transfer rod through the sample transfer rod clamp, so that a sample in the vacuum sealing transfer box is transmitted into and taken back from a vacuum sample chamber of an electron microscope or a micro-nano laser processing system, and meanwhile, an insulating layer is arranged at the contact part of the sample transfer rod clamp and a base of the vacuum sealing transfer box.
6. The apparatus for sample sealing and vacuum transfer for cross-platform connection according to claim 1, wherein the magnetically coupled transfer pins are responsible for movement along the axial direction, and the mechanical portion of the magnetically coupled transfer pins is connected with the external controller of the transfer pins by non-mechanical contact, thereby achieving connection with the magnetically coupled transfer pins under high vacuum and displacement of the magnetically coupled transfer pins in three-dimensional space.
7. The device for sample sealing and vacuum transfer for cross-platform connection according to claim 1, wherein the vacuum sealing transfer box is provided with a vacuum sealing transfer box top cover, a sealing sample holder, a base, a Teflon rubber O ring and a clamping groove, the top of the base is provided with the sealing sample holder, the sample is placed on the sealing sample holder, the bottom of the base is provided with the clamping groove, the vacuum sealing transfer box top cover capable of being buckled with the base is arranged above the base, and the vacuum sealing transfer box top cover and the base are sealed through the Teflon rubber O ring; meanwhile, the top of the vacuum sealing transfer box top cover is provided with a mechanical arm unlocking mechanism connected with a rotary unlocking manual valve of the vacuum transition bin.
8. The device for sealing and transferring samples across a platform according to claim 7, wherein after the top cover of the vacuum sealed transfer box is opened, the device enters a vacuum sample chamber of an electron microscope or micro-nano laser processing system under the pushing of a magnetic coupling sample transmission rod and is in butt joint with a sample stage in the vacuum sample chamber through a clamping groove.
9. The device for cross-platform connection of sample sealing and vacuum transfer as claimed in claim 1, wherein a track for controlling the butt joint of the base and the sample stage in the vacuum sample chamber of the electron microscope or the micro-nano laser processing system is processed on the base of the vacuum sealing transfer box, so that the magnetic coupling sample transfer rod can realize the transfer butt joint after entering the vacuum sample chamber of the electron microscope or the micro-nano laser processing system, and the magnetic coupling sample transfer rod can be withdrawn into the vacuum pipeline of the sample transfer rod after the adjustment of the spatial position of the sample is completed.
10. The device for sealing and transferring the sample across the platform according to claim 1, wherein the device can effectively realize inert gas sealing and vacuum transfer of the sample to be analyzed and processed in a micro-scale mode between the glove box, the scanning electron microscope, the double-beam electron microscope and the micro-nano laser processing system across the platform, and realize microstructure and element intrinsic analysis.
Technical Field
The invention relates to a material testing technology, in particular to a sample sealing and vacuum transfer device for cross-platform connection of a glove box, a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system, and belongs to the field of electron microscopes or micro-nano laser processing system accessories and material microstructure testing and analysis.
Background
A double-beam electron microscope and a micro-nano laser processing system are important tools for high-precision processing, modification and forming of nano-micron scale structures of materials. By utilizing the processing function of the focused ion beam equipped by the double-beam electron microscope, the continuous high-precision preparation and forming of the structure from the near 10nm level to the micron level can be realized. And (3) utilizing an electron beam high-resolution microscopic characterization method in a scanning electron microscope and a double-beam electron microscope to further obtain the high-resolution microscopic morphology, the three-dimensional defect structure and the distribution information of the material on the nano-micron scale. And applying corresponding coupling environment fields (such as force, electricity/magnetism, temperature and the like) on the micro-scale structure and the sample by combining a corresponding electron microscope micro-control and loading device, and observing the micro-or microstructure evolution of the material in the relevant environment in situ.
Scanning electron microscopes, double-beam electron microscopes and micro-nano laser processing systems are widely applied to the aspects of traditional materials, advanced new materials, semiconductor materials, nanotechnology, catalytic materials and the like, direct fine processing and high-resolution characterization of magnetic materials, low-dielectric-coefficient materials, biological/medical materials, polymer composite materials and ceramic materials are achieved, great potential is shown in the fields of new materials, environment, energy, chemistry and the like, and the problems of transfer, pollution and oxidation of samples still exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a sample sealing and vacuum transfer device for cross-platform connection of a glove box, a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system, so that cross-platform sealing and vacuum transfer of a sample to be analyzed and micro-processed in the double-beam electron microscope or the micro-nano laser processing system are realized to the maximum extent, and three-dimensional displacement control and butt joint of the sample in a sample bin are realized.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a sample sealing and vacuum transfer device for cross-platform connection, comprising: the device comprises a rectangular airtight flange, a vacuum transition bin, a bin door, a sample transfer rod vacuum pipeline, a sample transfer rod external controller, a manual rotating unlocking valve, a magnetic coupling sample transfer rod, a vacuum seal transfer box, a sample transfer rod clamp and an observation window, wherein the rectangular airtight flange is used for connecting a vacuum sample chamber and the vacuum transition bin of an electron microscope or a micro-nano laser processing system, the vacuum transition bin is used for placing and replacing a vacuum seal transfer box, the bin door is used for observing opening, the sample transfer rod vacuum pipeline, the sample transfer rod external controller, the manual rotating unlocking valve is used for magnetically coupling the sample transfer rod, the vacuum:
the vacuum transition bin is of a five-channel structure with a front channel, a rear channel, a left channel, a right channel and an upper channel, and a flange is arranged at the port of each channel; the port parts of the front channel and the rear channel of the vacuum transition bin are respectively provided with a bin door and an observation window, the bin door is hermetically connected with the front channel of the vacuum transition bin through a flange, and the observation window is hermetically connected with the rear channel of the vacuum transition bin through a flange; a flange at the port of a left channel of the vacuum transition bin is a rectangular airtight flange; a sample transfer rod vacuum pipeline is arranged at the right channel port of the vacuum transition bin and is hermetically connected with the right channel of the vacuum transition bin through a flange; a rotary unlocking manual valve is installed at the port of an upper channel of the vacuum transition bin, and the rotary unlocking manual valve is hermetically connected with the upper channel of the vacuum transition bin through a flange;
one end of the magnetic coupling sample transfer rod penetrates through the left channel and the right channel of the vacuum transition bin, is matched with a slide way in the sample transfer rod vacuum pipeline and slides in the sample transfer rod vacuum pipeline in a reciprocating manner; the sample transfer rod external controller is arranged on the sample transfer rod vacuum pipeline, the magnetic coupling sample transfer rod and the sample transfer rod external controller realize non-contact connection in a magnetic coupling mode, and the magnetic coupling sample transfer rod realizes displacement control through the sample transfer rod external controller; the other end of the magnetic coupling sample transfer rod is provided with a sample transfer rod clamp, and the vacuum sealing transfer box is arranged on the sample transfer rod clamp.
The device is characterized in that a sample sealing and vacuum transferring device for cross-platform connection is arranged, a left channel of a vacuum transition bin is connected with the side wall of a vacuum sample chamber of an electron microscope or a micro-nano laser processing system through a matched vacuum rubber ring and a rectangular airtight flange, and a right channel of the vacuum transition bin is connected with a matched sample transfer rod vacuum pipeline and a sample transfer rod external controller.
The rectangular airtight flange is a variable cross-section flange, one side of the rectangular airtight flange is connected with the side wall of a vacuum sample chamber of an electron microscope or a micro-nano laser processing system, the area of the rectangular airtight flange is relatively large, the other side of the rectangular airtight flange is communicated with the side wall of a vacuum transition bin, and the rectangular airtight flange is relatively small in diameter in order to adapt to the size and guarantee the sealing performance of the rectangular airtight flange.
The vacuum transition bin is provided with an openable bin door, and the bin door is sealed and locked on the vacuum transition bin through a vacuum caliper.
The sample sealing and vacuum transferring device for cross-platform connection is characterized in that a sample transfer rod clamp fixes the relative position of a vacuum sealing transferring box in the moving process and the opening process of a top cover of the vacuum sealing transferring box, the vacuum sealing transferring box enters a vacuum transition bin under the driving of a magnetic coupling sample transfer rod, and the vacuum sealing transferring box is installed and taken out after a bin door of the vacuum transition bin is opened; the vacuum sealing transfer box is connected with the magnetic coupling sample transfer rod through the sample transfer rod clamp, so that a sample in the vacuum sealing transfer box is transmitted into and taken back from a vacuum sample chamber of an electron microscope or a micro-nano laser processing system, and meanwhile, an insulating layer is arranged at the contact part of the sample transfer rod clamp and a base of the vacuum sealing transfer box.
The sample sealing and vacuum transferring device for cross-platform connection is characterized in that the magnetic coupling sample transfer rod is in charge of moving along the axis direction, and the mechanical part of the magnetic coupling sample transfer rod is connected with the sample transfer rod external controller in a non-mechanical contact manner, so that the connection with the magnetic coupling sample transfer rod under high vacuum and the displacement of a three-dimensional space of the magnetic coupling sample transfer rod are realized.
The vacuum seal transfer box is provided with a vacuum seal transfer box top cover, a seal sample holder, a base, a Teflon rubber O ring and a clamping groove, the top of the base is provided with the seal sample holder, a sample is placed on the seal sample holder, the bottom of the base is provided with the clamping groove, the vacuum seal transfer box top cover which can be buckled with the base is arranged above the base, and the vacuum seal transfer box top cover and the base are sealed through the Teflon rubber O ring; meanwhile, the top of the vacuum sealing transfer box top cover is provided with a mechanical arm unlocking mechanism connected with a rotary unlocking manual valve of the vacuum transition bin.
The sample sealing and vacuum transferring device for cross-platform connection is pushed by a magnetic coupling sample transmission rod to enter a vacuum sample chamber of an electron microscope or a micro-nano laser processing system after a top cover of a vacuum sealing transferring box is opened, and is in butt joint with a sample table in the vacuum sample chamber through a clamping groove.
The sample sealing and vacuum transferring device for cross-platform connection is characterized in that a track for controlling the butt joint of a base and a sample platform in a vacuum sample chamber of an electron microscope or a micro-nano laser processing system is processed on the base of a vacuum sealing transferring box, so that the magnetic coupling sample transferring rod is in transfer butt joint after entering the vacuum sample chamber of the electron microscope or the micro-nano laser processing system, and the magnetic coupling sample transferring rod is withdrawn into a sample transferring rod vacuum pipeline after the spatial position of a sample is adjusted.
The device can effectively realize the cross-platform inert gas sealing and vacuum transfer of the sample to be analyzed and micro-scale processing between the glove box, the scanning electron microscope, the double-beam electron microscope and the micro-nano laser processing system, and realize the intrinsic analysis of a microstructure and elements.
The design idea of the invention is as follows:
in order to solve the prominent problems commonly existing in the prior art, the applicant invents a sample sealing and vacuum transfer device for cross-platform connection of an electron microscope or micro-nano laser processing system based on a work foundation which is consolidated in the field for many years, the invention can realize that a sample to be analyzed and processed is placed above a sealed sample holder in an inert gas environment glove box or a vacuum environment for fixation, the sealed sample holder is inserted into a sample platform of a vacuum sealed transfer box, a top cover of the vacuum sealed transfer box is screwed after the fixation, the vacuum sealed transfer box is placed on a top clamp of a magnetic coupling sample transmission rod of a vacuum transition bin, the vacuum sealed transfer box can be directly inserted into a focused ion beam double-beam electron microscope and a micro-nano laser processing system for micro-scale processing or inserted into a scanning electron microscope for micro-area analysis with different functions, and effectively avoids the sample from being converted among different electron microscopes or micro-nano laser processing systems, the problems of sample damage, water and air pollution, oxidation and the like are caused, the microscale processing and microstructure analysis of the sample are greatly facilitated, the data and characterization reliability and the working efficiency are improved, and the method is widely applicable to the connection of scanning electron microscopes, double-beam electron microscopes or micro-nano laser processing systems.
The invention has the advantages and beneficial effects that:
1. the device can effectively realize the sealing and vacuum transfer loading of a sample to be analyzed among a glove box, a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system cross platform, and realize the intrinsic analysis of a microstructure. The device can realize water and air pollution isolation and atmosphere or vacuum protection transfer, can meet the requirements of characterization of electron beams, ion beams, laser and microbeam processing in an electron microscope or micro-nano laser processing system, realizes the accuracy of microstructure intrinsic branches, analysis and test results, and has the transfer vacuum degree of less than or equal to 2 multiplied by 10-3Pa。
2. According to the invention, by selecting the sealing sample holder with a proper angle control, the tilting angle range of the sample in the scanning electron microscope and the double-beam electron microscope can be 0-70 degrees, and the experimental test contents of electron back scattering diffraction and the like in the scanning electron microscope and the double-beam electron microscope can be met.
Drawings
FIG. 1 is an effect diagram of a sample sealing and vacuum transfer device for cross-platform connection of an electron microscope or micro-nano laser processing system.
Fig. 2 is a schematic view of the vacuum-tight transfer box installation and opening.
FIG. 1 illustrates the following: the vacuum transfer device comprises a rectangular airtight flange 1, a
FIG. 2 illustrates the following: 4 sample transfer rod vacuum pipelines, 6 rotating unlocking manual valves, 8-1 vacuum sealing transfer box top covers, 8-2 sealing sample holders, 8-3 bases, 8-4 Teflon rubber O rings, 8-5 clamping grooves and 13 mechanical arm unlocking mechanisms.
Detailed Description
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings and examples. With respect to the detailed description of these embodiments, it is to be understood that one skilled in the art can practice the invention and that other embodiments may be utilized and that changes and/or modifications may be made to the illustrated examples without departing from the spirit and scope of the appended claims. In addition, although specific features of the invention are disclosed in the embodiments, such specific features can be modified as appropriate to achieve the functions of the invention.
As shown in fig. 1-2, the cross-platform connected sample sealing and vacuum transfer device of the electron microscope or micro-nano laser processing system of the invention mainly comprises: a rectangle airtight flange 1 for connecting scanning electron microscope, two bunch of electron microscopes or receive vacuum sample room and the vacuum transition bin of laser processing system a little, a
the
The left channel of the
One end of the magnetic coupling
The other end of the magnetic coupling
The vacuum
A track for controlling the butt joint of the base 8-3 and a sample platform in a vacuum sample chamber of a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system is processed on the base 8-3 of the vacuum
The working process of the invention is as follows:
the invention can realize the atmosphere sealing and vacuum transfer of a microstructure test and a surface analysis sample among a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system, after the sample to be processed, analyzed and characterized is placed above a sealing sample holder 8-2 of a vacuum
The method comprises the steps of placing a test sample on a sealing sample holder 8-2 of a vacuum
The result shows that the device can effectively realize inert gas sealing and vacuum transfer of the sample to be analyzed and processed in a microscale between cross platforms of a glove box, a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system, and realize the intrinsic analysis of a microstructure and elements. The device can realize the protection transfer of water and air pollution-proof environment and atmosphere, and the transfer vacuum degree is less than or equal to 2 multiplied by 10-3Pa, can meet the requirements of characterization of electron beams, ion beam and laser and microbeam processing in a scanning electron microscope, a double-beam electron microscope or a micro-nano laser processing system.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
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