阅读说明：本技术 一种stm-mbe联用系统 (STM-MBE combined system ) 是由 姚杰 单欢 毛亚会 翟晓芳 赵爱迪 于 2020-07-02 设计创作，主要内容包括：本发明公开了一种STM-MBE联用系统,包括进样腔体、样品制备腔体、样品表征腔、支撑台以及烘烤系统。其中表征腔是直接购买的商用STM进样腔,可以实现在进样腔内很好的对样品进行解离、转移、以及沉积一些易污染真空的小分子。制备腔采用了预留下置圆形对称排列的窗口用于放置蒸发源,一次同时可以放置七个蒸发源,另外制备腔体采用了分子泵直接安装于离子泵后面的方式,可以实现分子泵对制备腔体的直抽,提高制备腔体的真空度,同时制备腔体预留了相比于以往的制备腔体,预留了更多的窗口,使其具有更多升级的空间,以及根据实验需要变化的可能性。烘烤系统,采用了外置进样腔的烘烤模式,且烘烤板采用双开门设计易于拆卸安装。具有更多的自我组装空间。(The invention discloses an STM-MBE (STM-MBE) combined system which comprises a sample injection cavity, a sample preparation cavity, a sample characterization cavity, a supporting table and a baking system. The characterization cavity is a commercial STM sample injection cavity which is directly purchased, and can realize dissociation, transfer and deposition of some small molecules which easily pollute vacuum in the sample injection cavity. The preparation cavity adopts the reserved windows which are arranged circularly and symmetrically and are arranged below the preparation cavity for placing evaporation sources, seven evaporation sources can be placed at the same time, in addition, the preparation cavity adopts the mode that the molecular pump is directly arranged behind the ion pump, the molecular pump can directly pump the preparation cavity, the vacuum degree of the preparation cavity is improved, and meanwhile, compared with the traditional preparation cavity, the preparation cavity is reserved with more windows, so that the preparation cavity has more upgraded space and the possibility of changing according to the experimental requirements. The baking system adopts a baking mode of an external sample feeding cavity, and the baking plate adopts a double-door design and is easy to disassemble and assemble. Has more self-assembly space.)

1. The utility model provides a STM-MBE allies oneself with system, includes five parts, is baking plate (1-1), sign chamber (1-2), preparation chamber (1-3), advances kind chamber (1-4), shelf (1-5) respectively, its characterized in that: the baking plate (1-1) is composed of 7 blocks in total, wherein a third heat insulation plate (7-3) and a fourth heat insulation plate (7-4) are in a hole-digging splicing type, the third heat insulation plate (7-3) and the fourth heat insulation plate (7-4) form a side surface together, a sixth heat insulation plate (7-6) on the outer side and a seventh heat insulation plate (7-7) on the inner side form a whole together, and a small hole is formed in the sixth heat insulation plate (7-6) and used for wiring in the baking process; the first heat insulation plate (7-1), the second heat insulation plate (7-2), the third heat insulation plate (7-3) and the fifth heat insulation plate (7-5) are all a whole to form a side surface, and the clapboards are fastened and connected by adopting a lock catch;

an ion pump (2-1), a mechanical arm (4-1-1), an argon gun (4-2-1), a low-energy electron diffraction gun (4-9-1), a low-energy electron diffraction screen (4-13-1), a film thickness meter (4-11-1), an access magnetic transmission rod (4-12-1), an alkali metal source (4-15-1), a quick-release evaporation source system (4-17-1), a titanium pump (4-20-1), an infrared thermometer (5-1-1), a camera (5-3-1), a three-dimensional table (4-10-1), an evaporation source (5-2-1), an evaporation source (5-4-1), an evaporation source (5-6-1) and the like are connected to the preparation cavity (1-3), An evaporation source (5-7-1) and an evaporation source (5-8-1);

the preparation cavity (1-3) is fixed with the frame (1-5) through four evenly distributed bearing ears and trapezoidal connecting pieces by using a screw rod and a screw cap of M20;

the rear end of the ion pump (2-1) is directly connected with the pneumatic valve (2-3), and the molecular pump (2-4) is connected behind the pneumatic valve (2-3), so that the molecular pump (2-4) and the ion pump (2-1) can directly pump the preparation cavity (1-3);

a manipulator (3-1-1), a quick opening door (3-2-1), a gas steel cylinder (3-5-1) with a micro-leakage valve, a pipeline (3-6-1) with a needle valve, a vacuum agent (3-7-1), a sampling bottle (3-8-1) with a micro-leakage valve, a quadrupole mass spectrometer (3-3-1), a transmission rod (3-9-1) and a small molecular pump (3-4-1) are connected to the sample injection cavity (1-4);

the head of the transmission rod (3-9-1) is provided with two sample grooves which are stacked.

2. An STM-MBE coupling system according to claim 1, wherein: one side of the baking plate (1-1) adopts a double-door design, and the sample injection cavity (1-4) is not in the coverage range of the baking plate (1-1).

3. An STM-MBE coupling system according to claim 2, wherein: the sample injection cavity (1-4) is connected with a small molecular pump (3-4-1) which can be independently vacuumized to keep the independent integrity.

4. An STM-MBE coupling system according to claim 3, wherein: the preparation cavity (1-3) is designed by an upper manipulator (3-1-1), and the head sample groove of the transmission rod (3-9-1) is designed by a double-layer sample rack, so that two samples can be transmitted simultaneously.

5. An STM-MBE coupling system according to claim 4, wherein: the preparation chambers (1-3) adopt a design mode that the bottom can be integrally detached, and the evaporation sources on the preparation chambers are arranged in a downward mode and are arranged in a circle.

6. An STM-MBE coupling system according to claim 5, wherein: the preparation cavity (1-3) adopts a mode that the ion pump (2-1) is arranged on the side surface, and the molecular pump (2-4) is connected behind the ion pump.

7. An STM-MBE coupling system according to claim 6, wherein: the ion pump (2-1) is supported by a special ion pump support (1-11), the support height of the ion pump can be adjusted, and the small molecule pump (3-4-1) is supported by a special molecular pump support (1-12), and the support height of the small molecule pump can be adjusted.

8. An STM-MBE coupling system, which is characterized in that: the device comprises a sample introduction cavity, a preparation cavity, a representation cavity, a support table and a baking system, wherein a molecular pump is connected to the sample introduction cavity right below the sample introduction cavity and used for pumping vacuum of the sample introduction cavity, the lateral surface of the sample introduction cavity is connected with the preparation cavity in the horizontal direction through a gate valve, and the preparation cavity is connected with the representation cavity through the gate valve and an adjustable corrugated hose; the characterization cavity is directly fixed on the support table through a base meter screw, the preparation cavity is connected and fixed with the support table through four specially designed trapezoidal supports and a screw rod and a screw cap of M20, the sample injection cavity is supported by a molecular pump supported on the sample injection cavity through a supporting rod with adjustable height, and the ion pump of the preparation cavity is supported by a specially designed table with adjustable height;

the sample injection cavity adopts a mode of independently pumping vacuum by using a molecular pump, so that the sample injection cavity has better independence, and has more connecting openings and more functions than the traditional sample injection cavity. The sample feeding cavity is characterized in that a transfer cavity position is reserved right above the sample feeding cavity, a position interface of a cleavage rod is reserved on the side face of the sample feeding cavity, so that a sample can be cleaved in vacuum in the sample feeding cavity, the position of a vacuum gauge, the position of air release and the interface of the position of a quadrupole mass spectrometer are reserved, an evaporation source is added on the sample feeding cavity according to experimental needs, and the growth of the sample is realized in the sample feeding cavity, and compared with the traditional sample feeding cavity, the sample feeding cavity has stronger functions, higher vacuum degree, stronger independence and more superior upgrading and transforming space, so that the experimental needs are better met;

the preparation cavity comprises two parts, namely a cavity body with a large flange at the bottom and a lower opening, wherein the flange at the bottom is provided with eight openings in total, the centers of seven openings form a circle, in order to meet the requirements of different evaporation sources, two of the interfaces are designed to be CF63 interfaces, the rest 5 are common CF35 interfaces, and the middle of the bottom is also provided with a CF63 interface for connecting a camera to observe the condition in the cavity; the top of the cavity with the lower opening is provided with three openings, the opening in the middle is used for assembling the mechanical arm, the method for arranging the mechanical arm can perfectly solve the problem of taking samples from two conveying rods respectively, and the two openings, one for installing an argon gun and the other for serving as an observation window, are arranged on the top of the cavity with the lower opening in a laterally symmetrical mode; in addition, the side surface of the cavity with the lower opening is also reserved with an opening for high-energy electron diffraction, an alkali metal source interface, a vacuum gauge interface, an observation window and the like, wherein the side surface is also provided with a CF150 flange port for connecting an ion pump, and the rear end of the ion pump is directly connected with a molecular pump, so that the available space on the cavity can be greatly saved, the single molecular pump interface is saved on the preparation cavity, and in addition, the direct pumping mode of the molecular pump is adopted, so that the pumping efficiency and the vacuum degree are greatly improved; the supporting table is matched with the overall instrument system, and the side and the bottom of the overall instrument system are covered by aluminum plates by adopting an I-shaped steel framework;

baking system has adopted the baking mode in external appearance chamber for baking efficiency can improve, has reduced unnecessary and has toasted moreover, even make during baking system, appearance chamber also can the autonomous working, is used for dissociating the preparation sample operation, save time, baking system's board has one side to have adopted the design of two opening the door, and this one side is the one side of taking after a left side, and this makes the access board toast and makes more convenient and fast convenience, and this kind of design of two opening the door makes the gap department of two doors each symmetrically open half a circle, can just in time block in the junction of molecular pump and ionic pump and transfer link, be convenient for more installation and dismantlement.

Technical Field

The invention belongs to the field of ultrahigh vacuum equipment, and particularly relates to an STM-MBE (scanning tunneling microscope-moving bed) combined system.

Background

In recent years, as the influence of low-dimensional materials on electronic devices becomes more and more prominent, the research on the surface structure and the surface interface of the low-dimensional materials is more and more emphasized. Whereas Scanning Tunneling Microscopy (STM) plays an important role therein. In the study of low-dimensional materials, Molecular Beam Epitaxy (MBE) is generally used for synthesizing the low-dimensional materials, and then STM is used for characterizing and studying the low-dimensional materials. The interior of the STM-MBE combined system needs to be operated under an ultrahigh vacuum environment. Depending on the range of vacuum levels, a rough vacuum (10) is usually used⁵-10³Pa), low vacuum (10)³-10^-1Pa), high vacuum (10)^-1-10^{- 6}Pa), ultra-high vacuum (10)^-6-10^-10Pa) and very high vacuum: (<10^-10Pa) is added. Under ultrahigh vacuum, gas molecules and other small molecules can be well isolated from polluting the surface of the low-dimensional material, and the property of the surface interface of the low-dimensional material can be better researched. As low-dimensional materials play an important role in the development of high-tech materials, the need for developing ultrahigh vacuum equipment for researching low-dimensional materials becomes more urgent.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a novel ultrahigh vacuum, scanning tunnel microscope and molecular beam epitaxy combined system which is more reasonable in layout, has larger adjustable space and is higher in efficiency.

The technical scheme adopted by the invention is as follows:

an STM-MBE coupling system comprises five parts, namely a baking plate, a representation cavity, a preparation cavity, a sample injection cavity and a frame, wherein the baking plate comprises 7 blocks, a third heat insulation plate and a fourth heat insulation plate are in a hole digging splicing type, the third heat insulation plate and the fourth heat insulation plate jointly form a side surface, the sixth heat insulation plate on the outer side and the seventh heat insulation plate on the inner side jointly form a whole, and a small hole is formed in the sixth heat insulation plate and used for wiring in the baking process; the first heat insulation plate, the second heat insulation plate, the third heat insulation plate and the fifth heat insulation plate are all integrated to form a side surface, and the partition plates are fastened and connected by adopting a lock catch;

an ion pump, a mechanical arm, an argon gun, a low-energy electron diffraction screen, a film thickness meter, a magnetic transmission rod, an alkali metal source, a quick-release evaporation source system, a titanium pump, an infrared thermometer, a camera, a three-dimensional table, an evaporation source and an evaporation source are connected to the preparation cavity;

the preparation cavity is fixed with the frame through four evenly distributed bearing ears and a trapezoidal connecting piece by using a screw rod and a screw cap of M20;

the rear end of the ion pump is directly connected with the pneumatic valve, and the molecular pump is connected behind the pneumatic valve, so that the molecular pump and the ion pump can directly pump the preparation cavity;

the sample injection cavity is connected with a mechanical arm, a quick opening door, a gas steel cylinder with a micro-leakage valve, a pipeline with a needle valve, a vacuum agent, a sampling bottle with a micro-leakage valve, a quadrupole mass spectrometer, a transmission rod and a small molecular pump;

the head of the conveying rod is provided with two sample grooves which are stacked.

Furthermore, one side of the baking plate adopts a double-door design, and the sample injection cavity is not covered in the baking range.

Furthermore, the sample injection cavity is connected with a small molecular pump, which can be independently vacuumized to keep the independent integrity.

Furthermore, the preparation cavity is designed to be provided with an overhead manipulator, and the head sample groove of the transmission rod is designed to be a double-layer sample rack, so that two samples can be transmitted simultaneously.

Furthermore, the preparation cavity adopts a design mode that the bottom can be integrally disassembled, and the upper evaporation source adopts a downward arrangement mode and is arranged in a circumference mode.

Furthermore, the preparation cavity adopts a mode that an ion pump is arranged on the side surface, and a molecular pump is connected behind the ion pump.

Furthermore, the ion pump is supported by a special ion pump support, the support height of the ion pump can be adjusted, and the small molecule pump is supported by a special molecule pump support, and the support height of the small molecule pump can be adjusted.

An STM-MBE combined system comprises a sample injection cavity, a preparation cavity, a representation cavity, a support table and a baking system. The sample injection cavity is connected with a molecular pump right below the sample injection cavity and used for extracting vacuum of the sample injection cavity, the lateral surface of the sample injection cavity is connected with the preparation cavity in the horizontal direction through a gate valve, and the preparation cavity is connected with the characterization cavity through the gate valve and the adjustable corrugated hose. The sign chamber is through the rice screw snap-on in the brace table, and the preparation cavity is connected fixedly with the brace table through the trapezoidal support of four special designs and with M20's screw rod and nut, and the sample introduction chamber supports through the molecular pump that supports on it with adjustable height's bracing piece. The ion pump for preparing the cavity is supported by a specially designed table with adjustable height.

Advance the appearance cavity, adopted the mode of using the molecular pump to draw the vacuum alone, this lets it have better independence, just it advances the appearance cavity and has more connection opening and function than the tradition advances the appearance cavity, has reserved the transfer chamber position directly over it, the position interface of cleavage stick has been reserved to the side, can realize advancing the appearance intracavity and carry out the vacuum cleavage to the sample, and still reserved the position of vacuometer, the position of gassing and the interface of quadrupole mass spectrometer position, this kind of design in addition, can be according to the experiment needs, add the evaporation source on advancing the appearance cavity, the growth to the sample is realized advancing in the appearance cavity. The sample injection cavity has more powerful functions, higher vacuum degree, stronger independence and more superior upgrading and transformation space compared with the traditional sample injection cavity, and meets the requirements of experiments more.

The preparation cavity comprises two parts, namely a cavity body with a large flange at the bottom and a lower opening, wherein the flange at the bottom is provided with eight openings in total, the centers of seven openings form a circle, in order to meet the requirements of different evaporation sources, two of the interfaces are designed to be CF63 interfaces, the rest 5 are common CF35 interfaces, and the middle of the bottom is also provided with a CF63 interface for connecting a camera to observe the condition in the cavity. The cavity with the lower opening is provided with three openings at the top, the opening in the middle is used for assembling the mechanical arm, the method for arranging the mechanical arm can perfectly solve the problem of taking samples from two conveying rods respectively, and the two openings, namely the two openings outside the cavity with the laterally symmetrical top, are used for installing an argon gun and are used as an observation window. In addition, the side surface of the cavity with the lower opening is also reserved with an opening for high-energy electron diffraction, an alkali metal source interface, a vacuum gauge interface, an observation window and the like, wherein the side surface is also provided with a CF150 flange port for connecting an ion pump, and the molecular pump is directly connected at the rear end of the ion pump, so that the available space on the cavity can be greatly saved, the single molecular pump interface is saved on the preparation cavity, and in addition, the direct pumping mode of the molecular pump is adopted, so that the pumping efficiency and the vacuum degree are greatly improved. The supporting table is matched with the general instrument system, and the whole supporting table adopts an I-steel framework side and an aluminum plate cover for the bottom.

The baking system adopts a baking mode of the external sample injection cavity, so that the baking efficiency is improved, unnecessary baking is reduced, the sample injection cavity can also work independently even during the baking system, the sample injection cavity is used for dissociating and preparing samples and the like, and the time is saved. In addition, the board of baking system, one side has adopted the design of two opening doors, and this side is the one side of taking after left, and this makes the board of taking toast and makes more convenient, and this kind of design of two opening doors makes the gap department of two doors each open the semicircle symmetrically, can just in time block in the junction of molecular pump and ion pump and transfer bar, be convenient for more installation and dismantlement.

The principle of the invention lies in; this STM-MBE allies oneself with system belongs to the ultra-high vacuum equipment field, and the sample preparation and the surface characterization of concretely relates to ultra-high vacuum. The STM-MBE combined system has the functions of realizing integration of sample cleavage, sample growth, sample characterization and the like, and has more self-assembly space compared with the prior STM-MBE system. This novel STM-MBE instrument system can divide into four parts on the whole. The method comprises the following steps: the device comprises a sample introduction cavity, a sample preparation cavity, a sample characterization cavity and a supporting table. Where the characterized cavity is a commercial STM that we purchase directly, the rest are self-designed and manufactured. The sample injection cavity body is compared with the previous sample injection cavity body, more functions are given to the sample injection cavity body, in the system, the sample injection cavity body is independently vacuumized through the molecular pump, the cavity body can be endowed with more excellent vacuum degree, and the designed sample injection cavity body can realize that a sample is well dissociated, transferred and deposited in the sample injection cavity body, so that small molecules which are easy to pollute the vacuum are obtained. The preparation cavity is characterized in that windows which are arranged in a reserved circular and symmetrical mode are used for placing evaporation sources, seven evaporation sources can be placed at the same time, in addition, the preparation cavity adopts a mode that a molecular pump is directly installed behind an ion pump, the molecular pump can directly pump the preparation cavity, the vacuum degree of the preparation cavity is improved, and meanwhile, compared with the traditional preparation cavity, more windows are reserved in the preparation cavity, so that the preparation cavity has more upgraded space and the possibility of changing according to experimental needs. The supporting table is a light and high-strength design designed according to the requirements and fastening principles of an instrument system. In addition, the system specially upgrades the baking system, adopts the baking mode of an external sample feeding cavity, improves the baking efficiency, avoids unnecessary baking, does not influence the preparation of some basic samples in the sample feeding cavity due to the independence of the sample feeding cavity during baking, and greatly saves time.

Compared with the prior art, the invention has the following remarkable advantages:

(1) the design of the upper manipulator is adopted on the preparation cavity, the special requirement that the manipulator with the rotary clamping is required for the transmission rod of the sample injection cavity is released, so that the sample rack of the transmission rod can be upgraded and reformed to be a double-layer sample rack, two samples can be transmitted simultaneously, and the efficiency is greatly improved.

(2) Function is abundanter on the appearance cavity of advancing, and we carry out the evacuation to advancing the appearance chamber with the molecular pump alone moreover for it is more independent and advance the vacuum in appearance chamber higher to advance the appearance chamber, does not influence the use that advances the appearance chamber when making the whole stoving of instrument system, and because the interface in appearance chamber compares existing design, more reasonable, the quantity is more. So that the space for modification and upgrading according to the experimental needs is larger. For example: the sample introduction cavity can be transformed, and experiments for introducing hydrogen and water or other experiments with strong pollution vacuum degree can be performed in the sample introduction cavity. Based on the small, flexible and easy-to-clean property of the sample feeding cavity and the independence of the sample feeding cavity, the phenomenon that the vacuum degree is reduced due to pollution of the whole system can be isolated.

(3) On the preparation chamber, we have adopted the design mode that can wholly dismantle the bottom, be convenient for more to the inside cleanness and the maintenance of cavity. In addition, the evaporation sources are arranged in a circular mode in a downward mode, so that the space is saved, and more evaporation sources can be placed at one time. The bottom, the side and the top are provided with observation windows, and all the inside of the cavity can be observed in 360 degrees without dead angles. The preparation cavity has more complete and powerful functions, and can be simultaneously provided with a high-energy electron diffraction device (REED), a manipulator, direct current heating, an infrared thermometer, an alkali metal source and the like. In addition, the ion pump is arranged on the side face, and the molecular pump is connected to the back of the ion pump, so that the cavity can be directly pumped by the molecular pump, the vacuum pumping efficiency is improved, the design that the molecular pump needs to be connected to the cavity in another position is eliminated, and the space utilization rate of the cavity is greatly improved. Finally, compared with the existing scanning tunnel microscope and molecular beam epitaxy evaporation instrument system, the preparation cavity has more reasonable interface arrangement and more interfaces, so that the space for modifying and upgrading the preparation cavity according to the experimental needs is huge.

(4) Baking systems, we upgrade compared to the prior art. Based on the independence of the sample injection cavity, the baking design of the external sample injection cavity is adopted, in addition, in order to facilitate the building and the dismounting of the baking plate, one side of the final assembly is provided with a double-door design, the position of the conveying rod and the position of the molecular pump are avoided due to the ingenious design, the building and the dismounting are more convenient, and the built baking tent is made to be more integrated as compared with the method that a part of baking cloth is additionally arranged in the previous requirement.

Drawings

FIG. 1 is a schematic diagram of the overall structure of the present invention;

FIG. 2 is a top view of the overall structure of the present invention;

FIG. 3 is a right side view of the overall construction of the present invention;

FIG. 4 is an elevational view of the general construction of the present invention;

FIG. 5 shows a trapezoidal shaped connector for a cavity and a frame according to the present invention;

FIG. 6 is a molecular pump support of the sample introduction chamber of the present invention;

FIG. 7 is a schematic view of an ion pump support of the fabrication chamber of the present invention;

FIG. 8 is a front view of a sample introduction chamber of the present invention;

FIG. 9 is a right side view of a sample introduction chamber of the present invention;

FIG. 10 is a block diagram of a transfer rod of the present invention;

FIG. 11 is a partial enlarged view of the head of the transfer rod of the present invention;

FIG. 12 is a formal drawing of a bare preparation cavity of the present invention;

FIG. 13 is a right side view of a bare preparation chamber of the present invention;

FIG. 14 is a bottom view of a bare preparation chamber of the present invention;

FIG. 15 is a top view of a bare preparation chamber of the present invention;

FIG. 16 is a front view of the assembled preparation chamber of the present invention;

FIG. 17 is a rear view of the assembled preparation chamber of the present invention;

FIG. 18 is a bottom view of the preparation chamber of the present invention fully assembled;

FIG. 19 is a top view of the assembled preparation chamber of the present invention;

FIG. 20 is a schematic view of the overall construction of the stand of the present invention;

FIG. 21 is a top view of the overall shelf construction of the present invention;

FIG. 22 is a partial perspective view of the overall construction of the shelf of the present invention;

figure 23 is an overall layout of the heat shield of the present invention.

Detailed Description

The invention is further described with reference to the following figures and detailed description.

Referring to fig. 1-22, an STM-MBE system includes five parts, as shown in fig. 1, a baking plate 1-1, a characterization chamber 1-2, a preparation chamber 1-3, a sample injection chamber 1-4, and a frame 1-5. The adjustable corrugated hoses 1-7 and the gate valves 1-8 are connected with each other. Characterization Chamber 1-2 was a mature commercial LT-STM plus Qplus-AFM function, available from scienta Omicron. The characterization chamber 1-2 is fixed with the frame 1-5 by a set screw, and the preparation chamber 1-3 is connected with and supported by an M20 screw nut and the frame 1-5 by four ladder supports 1-13. Detailed structural schematic diagrams of the trapezoidal supports 1-13 are shown in fig. 5, and fig. 5 is a structural schematic diagram of the trapezoidal supports at different angles.

The system realizes the ultrahigh vacuum of the vacuum system through four pump bodies, namely a mechanical pump, a molecular pump, an ion pump and a titanium pump. Firstly, a mechanical pump is connected with an upper molecular pump to pump rough vacuum for a vacuum system, then the system is further vacuumized through the molecular pump, and finally the system is enabled to reach ultrahigh vacuum through the ion pump and a titanium pump. The ion pump 2-1 of the preparation chamber shown in the figures 2, 3 and 4 is connected with the preparation chamber 1-3 through the opening of the CF150 at the side part of the preparation chamber, the back of the ion pump 2-1 is connected with the CF 150-CF 100 neck 2-2, the open end of the CF100 of the CF 150-CF 100 neck 2-2 is connected with a pneumatic valve 2-3, and the back of the pneumatic valve 2-3 is connected with the molecular pump 2-4 with the caliber of CF 100. An ion pump 2-1 of the preparation cavity is placed on an ion pump support 1-11, the specific structure of the ion pump support 1-11 is shown in figure 7, and four support columns are provided with threads, so that the height and the horizontal degree of a support surface can be conveniently adjusted by four feet at the bottom. An opening of CF63 at the lower part of the sample feeding cavity 1-4 is connected with a small molecular pump 2-5 with the caliber of CF63, and the lower part of the small molecular pump is supported by an adjustable support rod 1-12. The middle parts of the adjustable supporting rods 1-12 are screw rods, the supporting surfaces of the upper and lower parts are provided with internal threads for realizing height adjustment, and the specific structures of the adjustable supporting rods 1-12 are shown in figure 6.

Referring to fig. 8 and 9, the sample injection cavity system of the present system uses an independent small molecule pump 2-5 for vacuum pumping, and the sample injection cavity has 10 openings, and each opening is connected to a different functional part. The CF63 opening 3-1 is used to access the robot 3-1-1. Opposite the CF63 opening 3-1 is another CF63 opening 3-2 for accessing a quick opening door 3-2-1. CF35 opening 3-5, CF35 opening 3-6, CF35 opening 3-7, CF opening 3-8, two adjacent openings of four CF35 openings are vertical to each other and rotate 45 degrees with respect to the horizontal plane. The four openings are respectively connected with different functional parts, the CF35 opening 3-5 is connected with a gas steel cylinder 3-5-1 with a micro leakage valve, and a proper amount of hydrogen can be filled in the gas steel cylinder to meet the experiment requirement, and different gases can be switched in according to the specific experiment requirement. The opening 3-6 of the CF35 is connected with a pipeline 3-6-1 with a needle valve, and is used for realizing active air intake and vacuum breaking of the sample feeding cavity. The opening 3-7 of the CF35 is used for connecting a vacuum agent 3-7-1 and calibrating the vacuum degree in the sample feeding cavity. The opening 3-8 of the CF35 is used for connecting a sampling bottle 3-8-1 with a micro-leakage valve, and the interior of the sampling bottle can be filled with ultrapure water to meet the experimental requirement. The other group of openings are arranged near the CF63 opening 3-2, namely a CF35 opening 3-3, a CF35 opening 3-9, a CF35 opening 3-10 and a CF63 opening 3-4, wherein every two adjacent openings are vertical to each other. The CF63 opening 3-4 is centered on the same line as the CF35 opening 3-3, and its centerline is perpendicular to the horizontal. The opening 3-3 of the CF35 is connected with a quadrupole mass spectrometer 3-3-1 for leak detection of a vacuum system and analysis of element components in a vacuum cavity. The CF35 is provided with an opening 3-9 to be connected with the transmission rod 3-9-1, the specific structure of the transmission rod 3-9-1 is shown in figure 10, a partial enlarged view is shown in figure 11, the head part of the transmission rod 3-9-1 is provided with two sample grooves, two samples can be transmitted simultaneously, and the efficiency is greatly improved. The CF35 is connected with the preparation cavity through the opening 3-10 to realize the communication between the preparation cavity and the sample feeding cavity. The opening 3-4 of the CF63 is connected with a small molecular pump 3-4-1.

Referring to FIGS. 12, 13, 14 and 15, the unassembled preparation chamber 1-3 of the present system is composed of an upper part and a lower part, wherein the upper part has 20 openings, which are numbered consecutively from opening 4-1 to opening 4-20. The lower portion has a total of 8 openings, numbered consecutively from opening 5-1 to opening 5-8. The upper part and the lower part are connected through a huge flange of CF300, and the design facilitates the assembly and disassembly of the preparation cavities 1-3 and the cleaning work of the inner parts. And the four ears supporting the load of the preparation cavity are evenly distributed around the flange of the upper part, and two vertically arranged through holes of M20 are arranged in each ear for anchoring the preparation cavity 1-3.

In the preparation chamber 1-3, the center lines of five openings, i.e., the CF100 opening 4-9, the CF100 opening 4-13, the CF100 opening 4-15, the CF150 opening 4-19, and the CF35 opening 4-20, are all parallel to the horizontal plane. The centerlines of all openings except these five openings intersect at a point within the chamber, which is referred to as the center of the preparation chamber 1-3. The top end of the preparation cavity 1-3 is provided with three openings, on the same vertical plane I, a CF63 opening 4-3, a CF35 opening 4-2 and a CF100 opening 4-1 are respectively arranged, wherein the CF100 opening 4-1 is distributed in the middle of a circular plane at the top end of the preparation cavity 1-3, the openings of the CF63 opening 4-3 and the CF35 opening 4-2 are distributed on two sides, and the included angles between the opening center lines and the vertical direction are both 33 degrees. In addition, CF150 openings 4-19, CF35 openings 4-12, CF63 openings 4-8 and CF35 openings 4-16 are also on the same vertical plane I as CF63 openings 4-3, CF35 openings 4-2 and CF100 openings 4-1. And the opening centerlines of the CF35 openings 4-14, the CF35 openings 4-12, the CF100 openings 4-10 and the CF63 openings 4-8 are on the same plane II, and the plane II is perpendicular to the plane I. The centerline of the CF35 openings 4-12 is collinear with the centerline of the CF63 openings 4-8 at i, the centerline of the CF35 openings 4-14 is collinear with the centerline of the CF100 openings 4-10 at ii, and line i is perpendicular to line ii. CF100 opening 4-9 is collinear with the centerline of CF100 opening 4-13, iii. And the collinear line III is located at a distance of 1 cm below the plane II. The CF35 opening 4-4, the CF35 opening 4-5, the CF100 opening 4-6 and the CF63 opening 4-7 are all distributed on the cavity side wall of the preparation cavity 1-3 which is obliquely above the plane II. With opening 4-5 of CF35 being directly above opening 4-10 of CF 100. This opening is distributed below plane ii: CF35 openings 4-15, CF35 openings 4-16, CF35 openings 4-17, CF63 openings 4-18, CF150 openings 4-19, and CF100 openings 4-20. Wherein the CF35 openings 4-15, the CF150 openings 4-19 and the CF100 openings 4-20 are arranged, the central lines of the three openings are parallel to the horizontal plane, and the central lines of the remaining three openings pass through the centers of the preparation cavities 1-3. The lower part of the preparation chamber 1-3, 8 openings are distributed over the large flange of the CF 300. And the center lines of the 8 openings intersect at the center of the preparation chamber 1-3. The CF63 opening 5-3 was located at the very center of the bottom large flange, and the remaining seven openings were distributed in a circumferential array around the center with their centerlines all tilted 17 degrees from vertical.

Considering the bearing problem of the instrument system, reinforcing ribs are added to certain key necks in the system, such as the necks corresponding to the CF100 opening 4-1, the CF100 opening 4-10, the CF35 opening 4-14, the CF35 opening 3-9 and the CF35 opening 3-3. The wall thickness of the preparation cavity 1-3 is 5mm, and the thickness of the sample injection cavity 1-4 is 3 mm. In addition, in the system, the thickness of the neck where the CF150 flange and the CF100 flange are located is 3mm, the thickness of the CF63 flange neck is 2mm, the thickness of the corresponding neck is 2mm except for the CF35 openings 4-15 which adopt flange embedded connection, and the thickness of the rest CF35 flange necks is 1.6 mm.

With reference to FIGS. 16, 17, 18 and 19, the preparation chamber 1-3 of the present system is divided into upper and lower portions. In the upper part, a CF100 opening 4-1 is connected with a manipulator 4-1-1, a CF35 opening 4-2 is connected with an argon gun 4-2-1, a CF63 opening 4-3 is connected with a glass window 4-3-1, a CF35 opening 4-4 is connected with the glass window 4-4-1, a CF35 opening 4-5 is connected with a glass serial port 4-5-1, a CF100 opening 4-6 is connected with the glass window 4-6-1, a CF63 opening 4-7 is connected with the glass window 4-7-1, a CF63 opening 4-18 is connected with the glass window 4-18-1, and a CF63 opening 4-8 is connected with a CF63 gate valve 4-8-1, and the preparation cavity 1-3 is connected with a characterization cavity 1-2 through the gate valve. The CF100 opening 4-9 is connected with a low-energy electron diffraction gun 4-9-1, and the corresponding CF100 opening 4-13 is connected with a low-energy electron diffraction screen 4-13-1. The opening 4-10 of the CF100 is connected into a three-dimensional sample table 4-10-1, a sample can be heated on the sample by direct current, back bottom and electron beams, and meanwhile, a thermocouple is attached to the sample, so that the temperature of the sample can be measured. CF35 is connected to film thickness gauge 4-11-1 through opening 4-11. The opening 4-12 of the CF35 is connected with a magnetic transmission rod 4-12-1, the transmission rod 4-12-1 has the same structure and different length with the transmission rod 3-9-1 of the sample injection cavity 1-4, the specific structure of the transmission rod 4-12-1 is shown in figure 10, the partial enlarged view is shown in figure 11, and the head of the transmission rod 4-12-1 is also provided with two sample grooves, so that two samples can be transmitted simultaneously. The opening 4-14 of the CF35 is connected with a CF35 gate valve 4-14-1 and is responsible for communicating the preparation cavity 1-3 with the sample injection cavity 1-4. The CF35 is connected to a vacuum gauge 4-15-1 through an opening 4-15, and the degree of vacuum in the preparation chamber 1-3 is monitored. An opening 4-16 of CF35 is connected with an alkali metal source 4-15-1, an opening 4-17 of CF35 is connected with a small quick-release evaporation source system 4-17-1, the quick-release evaporation source system 4-17-1 is connected with a neck of CF 35-CF 63 through a CF35 opening 4-17 connected with a CF35 gate valve, then is connected with a tee with the caliber of CF63, is connected with a molecular pump on the side surface of the tee, and is connected with an evaporation source behind the tee. The quick-release evaporation source system 4-17-1 can realize quick replacement of the evaporation source required by the experiment under the condition of not damaging the vacuum of the preparation cavity 1-3. The opening 4-19 of the CF150 is connected with the ion pump 2-1, and the opening 4-20 of the CF100 is connected with the titanium pump 4-20-1. In the lower part of the preparation chamber 1-3, an opening 5-1 of CF63 is connected with an infrared thermometer 5-1-1, an opening 5-2 of CF35 is connected with an evaporation source 5-2-1, an opening 5-4 of CF35 is connected with an evaporation source 5-4-1, an opening 5-6 of CF35 is connected with an evaporation source 5-6-1, an opening 5-7 of CF35 is connected with an evaporation source 5-7-1, an opening 5-8 of CF35 is connected with an evaporation source 5-8-1, an opening 5-3 of CF63 is connected with a camera 5-3-1, the conditions of samples in the preparation chamber 1-3 are monitored, an opening 5-5 of CF63 is connected with a glass window 5-5-1, and of course, an opening 5-5 of CF63 can also be connected according to experimental requirements.

With reference to fig. 20, 21 and 22, the frames 1-5 of the system are rectangular frame structures, and the main frame is a hollow rectangular steel column, so that the system is light and high in strength. The upper surface of the frame 1-5 is characterized in that one side of the characterization cavity 1-2 is paved with a steel plate with the thickness of 5mm, one side of the preparation cavity 1-3 is supported by four hollow steel columns, the bottom surface of the frame 1-5 is provided with a steel plate with the thickness of 5mm, four side surfaces of the frame 1-5 are sealed by aluminum plates, and the aluminum plates are fixed by fastening screws. Thick heat insulation blankets are laid on the four side surfaces and the bottom surface of the shelves 1-5 for preventing heat from being diffused outwards. The rack 1-5 is provided with 5 heating sheets with fans, and the heating sheets 6-1, 6-2 and 6-5 are semi-fixed and can be taken down at any time when not baked. The heating plate 6-3 and the heating plate 6-4 are fixed heating plates.

Referring to fig. 23, the baking insulation panels of the present system are composed of 7 blocks in total, each made of hollow 304 stainless steel plate and filled with insulation cotton. The heat insulation plates 7-3 and 7-4 are in a hole-digging splicing type, and the two heat insulation plates jointly form a side surface, so that the integrity of the heat insulation plates is protected. The heat insulation plate 7-6 and the small heat insulation plate 7-7 together form a whole. And the heat insulation board 7-6 is provided with small holes for wiring in the baking process. The clapboards are fastened and connected by adopting a lock catch.

The operation of the ultra-high vacuum STM-MBE combined system comprises the following steps:

the method comprises the following steps: with reference to fig. 1, 2 and 3, the quick-release evaporation source system 4-17-1 is removed, the gate valve opened at 4-17 in the CF35 is sealed by a blind plate, and the gate valve is opened. Opening a gate valve 1-10 between a preparation cavity 1-3 and a sample injection cavity 1-4, closing a quick opening door 3-2-1 on the sample injection cavity 1-4, opening a gate valve 1-8 between the preparation cavity 1-3 and a characterization cavity 1-2, opening a pneumatic valve 2-3, then vacuumizing a molecular pump 2-4 on the preparation cavity 1-3 by using a mechanical pump, starting the molecular pump 2-4 after extracting to a certain vacuum degree, checking all vacuum gauge readings after extracting for 12 hours, and detecting the leakage by using a quadrupole mass spectrometer 3-3-1.

Step two: and (3) with reference to the figure 23, after the vacuum system is ensured to be leak-proof, closing the gate valve 1-10, closing the sample injection cavity vacuum gauge, placing all the heating sheets, and then starting to build a baking plate.

Step three: after baking for 48 hours, removing the baking plate, simultaneously beginning to degas the components in the system, after that, slowly introducing nitrogen from the air inlet valve 3-2-1, breaking the vacuum of the sample injection cavity 1-4, after the internal air pressure returns to the standard atmospheric pressure, opening the quick opening door 3-2-1, putting the sample injection product on the conveying rod 3-9-1, and because the conveying rod is provided with two sample grooves, two samples can be put in according to the experimental requirements. And closing the quick opening door 3-2-1, closing the air release valve, starting to vacuumize the sample injection cavity 1-4 by using the mechanical pump and the molecular pump 3-4-1, and opening a vacuum gauge of the sample injection cavity 1-4 to check the vacuum degree after pumping for 1 hour.

Step four: if necessary, the sample on the transmission rod can be clamped on the mechanical arm 3-1-1, the mechanical arm 3-1-1 is adjusted to enable the sample to reach a proper position, and a proper amount of gas such as hydrogen or water is introduced to the surface of the sample through the gas cylinder 3-5-1 with the micro-leakage valve and the gas cylinder 3-8-1 with the micro-leakage valve to meet the requirement of the experiment.

Step five: opening a gate valve 1-10 between the preparation cavity 1-3 and the sample injection cavity 1-4, communicating two vacuum cavities, transferring the transfer rod 3-9-1 carrying the sample into the preparation cavity 1-3, then clamping the sample by using a manipulator 4-1-1 of the preparation cavity 1-3, removing the transfer rod 3-9-1, moving the transfer rod 4-12-1 of the preparation cavity 1-3 to be right below the manipulator 4-1-1, transferring the sample from the manipulator 4-1-1 to the transfer rod 4-12-1, and transferring a second sample to the transfer rod 4-12-1 by using the same method if two samples exist. After the transfer is finished, the conveying rod 3-9-1 is moved back to the sample injection cavity 1-4, and the gate valve 1-10 is closed.

Step six: if there is excess sample. The sample can be transferred to the characterization chamber 1-2 for storage, leaving a sample of the substrate in the preparation chamber for processing. The sample on the transfer bar 4-12-1 is transferred to the three-dimensional stage 4-10-1 by the robot 4-1-1, and the substrate sample is placed at the center of the preparation chamber 1-4 by moving the three-dimensional stage 4-10-1. If the surface treatment is needed to be carried out on the sample, the three-dimensional table 4-10-1 can be rotated to enable the surface of the sample to be upward, then argon etching is carried out, heating annealing is carried out on the three-dimensional table, and cyclic treatment is carried out.

Step seven: if additional evaporation sources are needed during the material growth process, the CF35 opening 4-17 on the preparation chamber 1-3 can be accessed into the small fast-dismantling evaporation source system 4-17-1. Firstly closing a gate valve on a CF35 opening 4-17, then detaching a blind plate on the gate valve, then connecting a small quick-release evaporation source system 4-17-1, performing rough vacuum pumping on the quick-release evaporation source system 4-17-1 by using a mechanical pump after connection, and then starting a molecular pump of the quick-release evaporation source system 4-17-1 to perform vacuum pumping on the quick-release evaporation source system. After the vacuum is pumped for a period of time, the vacuum degree is observed through a vacuum gauge of the quick-release evaporation source system 4-17-1, and when the vacuum degree of the quick-release evaporation source system 4-17-1 is close to that of the preparation cavity 1-3, a gate valve between the two is opened, so that the quick-release evaporation source system 4-17-1 is communicated with the preparation cavity 1-3. The evaporation source in the quick-release evaporation source system 4-17-1 can be used after degassing.

Step eight: the material growth is carried out on the substrate, the three-dimensional table 4-10-1 can be rotated to enable the surface of the substrate sample to face downwards, then the evaporation source is utilized to carry out the material growth, and the growth condition of the material can be monitored by low-energy electron diffraction in the growth process. In the process, the sample can be heated by the three-dimensional table 4-10-1, and the temperature of the sample can be monitored doubly by the thermocouple on the three-dimensional table 4-10-1 and the infrared thermometer 5-1-1. The real-time specific conditions in the preparation cavity 1-3 can be detected by the camera 5-3-1 attached to the preparation cavity 1-3 in the whole process.

Step nine: and transferring the sample on the three-dimensional table to a transmission rod 4-12-1 by using a manipulator 4-1-1, opening a gate valve 1-8, communicating the characterization cavity 1-2 with the preparation cavity 1-3, and conveying the sample bed to the characterization cavity 1-2 by using the transmission rod 4-12-1 for characterization.

The above is only one embodiment of the present invention, but the scope of the present invention is not limited thereto. It should be noted that various changes and modifications to the present invention can be easily made by those skilled in the art without departing from the technical principle of the present invention, and those changes and modifications fall within the scope of the claimed invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.