CN211700186U - Integrated device for preprocessing transmission electron microscope sample and sample rod - Google Patents

Abstract

The utility model relates to the technical field of accessories for transmission electron microscopes, in particular to an integrated device for pretreatment of samples and sample rods of transmission electron microscopes. The device comprises: a plasma cleaning module, which is used for plasma cleaning of TEM samples; vacuum storage a module for vacuum storage of TEM samples and/or sample rods; a vacuum pump set capable of communicating with the plasma cleaning module and the vacuum storage module, respectively; and a valve assembly including a plurality of valves, which are The open and closed state of one or more of the plurality of valves allows the vacuum pump set to communicate with the plasma cleaning module and/or the vacuum storage module. The utility model can realize two kinds of pretreatments through a set of vacuum pump sets, saves parts, and avoids the possible risks such as falling off due to the need for excessive transfer of TEM samples between different independent devices.

Description

All-in-one unit for TEM sample and sample holder pretreatment

technical field

The utility model belongs to the field of scientific research instruments related to transmission electron microscopes, in particular to an integrated device for preprocessing a sample of a transmission electron microscope and a sample rod.

Background technique

Transmission Electron Microscope (TEM) uses an electron beam as a light source, and the concentrated and accelerated electron beam is incident on a thin sample, and the high-energy incident electrons interact with the sample to generate physical signals. The portion of the electrons that pass through the sample is called the transmitted electrons, and the transmitted electrons carry the intrinsic information of the sample. Since the thickness, atomic number, crystal structure, and orientation of the sample in each micro-region are different, the scattering angles of the transmitted electrons passing through the sample are not the same, thus forming different light and dark images that reflect the sample information. Due to the excellent spatial resolution of TEM, the micro- and nanoscale samples can be accurately characterized in terms of morphology, composition (EDS point, line, plane) and crystal structure (electron diffraction pattern, high-resolution image). Analytical characterization. Therefore, it is widely used in materials science, earth science, biological science and other fields and related research involving metals, alloys and semiconductors.

TEM experiments use electron beams to penetrate the sample to obtain the internal structure information of the sample, so the sample is extremely demanding. For example, the thickness of the sample must be less than 100nm. If high-resolution images are to be observed, the sample is required to be thinner, such as less than 50nm. . At present, the following two techniques are usually used to obtain TEM samples: 1) Such TEM samples can be prepared by conventional ion thinning method and electrolytic double jet method: diameter ≤ 3mm, thickness ≤ 100nm; 2) Using advanced focused ion beam technology (Focused Ion beam, FIB for short) can prepare such TEM flake samples: the length, width and thickness are usually about 10μm × 5μm × 0.1μm, and then bonded to a half-crescent-shaped TEM with a diameter of 3 mm and a thickness of about 30 μm TEM experiments were carried out on the metal carrier network. After the sample is prepared to the stage before the experiment, the surface needs to be kept flat and clean, free of contaminants and amorphous layers, in order to ensure the accuracy of the TEM experiment.

TEM1 is mainly composed of four parts: electron optical system, vacuum system, power supply system and operation control module. Referring to FIG. 1, FIG. 1 shows a working principle diagram of a TEM. As shown in FIG. 1 , the electron optical system mainly includes a top-down condenser lens 12 , a sample chamber 13 , an objective lens 14 , an intermediate mirror 15 , and a projection mirror 16 located in the vacuum lens barrel. After the filament in the electron gun 11 is heated, The electron beam is generated, and a very fine electron beam is formed after being focused by the two-stage condenser, and then further accelerated to penetrate the thin sample in the sample chamber. At this time, the transmitted electron beam carries the characteristic information of the sample, and then passes through the objective lens, The third-level magnification of the intermediate mirror and the projection mirror finally projects the information characterizing the sample onto the downstream phosphor screen 17, and takes pictures through the photographing room 18 to obtain the experimental results.

By inserting the lateral side of the sample rod loaded with the TEM sample into the sample chamber 13, the electron beam generated by the electron gun 11 at the top can be incident on the TEM sample to start the experiment. If gas molecules remain on the sample rod and enter the tube, high-speed electrons will collide with the remaining gas molecules, resulting in random electron scattering and difficulty in focusing, thereby affecting the resolution and imaging contrast of the TEM. In addition, the residual gas molecules may also accelerate the oxidation of the electron gun at the upstream end of the lens barrel, thereby shortening the service life of the electron gun. At the same time, the residual gas molecules will also contaminate the sample to a certain extent, affecting the acquisition of high-quality images. Therefore, it is necessary to maintain a good vacuum degree of the lens tube, so as to provide a good vacuum environment for the electron beam incident on the TEM sample. For example, for most TEMs, it is required to maintain a vacuum degree of 10 ^-7 -10 ^-11 Torr.

It can be seen that the TEM experiment has extremely high requirements on the integrity of the sample itself and the vacuum degree of the lens tube. However, during the current TEM experiment, the integrity of the sample itself and the sample rod inserted into the lens barrel will greatly interfere with the vacuum of TEM and the observation of TEM experiments. First, the prepared transmission samples are small in size, and their thickness is below 100 nm, or even thinner. It is very easy to interact with substances in the air to form hydrocarbon pollutants and organic pollution layers, and it is difficult to avoid them during storage. Second, place the samples. The sample rod is in the atmosphere when not in use, and the contact area with the air is large, and it is easy to adsorb water molecules, air and pollutants. Even if it is stored in a dry box, it cannot be avoided. After it enters the electron microscope, it will affect the lens tube The degree of vacuum will pollute the TEM objective lens, pole piece, diaphragm and filament, which will affect the experimental observation.

In response to the above problems, the following improvements have been made:

Document 1: US Patent Application (US5633502A) discloses a plasma processing method and apparatus, and the system can be used to clean the sample and the sample holder from contaminants.

Document 2: Chinese patent application (CN106783494A) discloses a vacuum storage and testing device for sample rods for transmission electron microscopes, which can effectively prevent the sample rods from being polluted or eroded when placed in the outside world and contaminate the electron microscope, and greatly shorten the sample rod in the electron microscope. The pre-pumping time is longer, so that the electron microscope can reach a stable vacuum degree faster and increase the service life of the sample holder.

It can be seen that (1) the equipment currently used to realize plasma cleaning and vacuum storage is an independent device with a single function. If the sample is switched multiple times, the sample and sample holder need to be transferred between different devices too much and across distances. Due to the extremely small size of the sample and the fragile sample holder, it may not only contaminate the sample and the sample during the transfer process. (2) Vacuuming-cleaning samples and vacuuming-vacuum storage of samples/sample rods should be carried out according to two independent devices, which not only operate efficiently low and extremely expensive.

Accordingly, a new technical solution is needed in the art to solve the above problems.

Utility model content

technical problem

In view of this, the technical problem to be solved by the present invention is how to perform pretreatment on the transmission electron microscope sample and the sample rod which is beneficial to the TEM experiment.

Technical solutions

The utility model provides an integrated device for pretreatment of a transmission electron microscope sample and a sample rod. The device comprises: a plasma cleaning module, which is used for plasma cleaning of a TEM sample; a vacuum storage module, which is used for cleaning the TEM sample. and/or sample rod for vacuum storage; a vacuum pump set capable of communicating with the plasma cleaning module and the vacuum storage module, respectively; and a valve assembly including a plurality of valves, by switching one of the plurality of valves or A plurality of open and closed states thereby communicate the vacuum pump set with the plasma cleaning module and/or the vacuum storage module.

For the above device, in a possible implementation manner, the plasma cleaning module includes a radio frequency power supply, a plasma generator and a cleaning chamber, a cleaning cavity is formed inside the cleaning chamber, and the oscillating field generated by the radio frequency power supply is excited into the plasma The process gas in the gas generator generates plasma, so as to clean the samples in the cleaning chamber, wherein the valve assembly includes a first valve, and the first valve is arranged on the vacuum pump group and the cleaning chamber so that the vacuum pump group is communicated with the cleaning chamber to perform vacuum extraction of the cleaning chamber when the first valve is opened.

For the above device, in a possible implementation manner, the cleaning chamber is provided with a plurality of inclined surfaces, each of the inclined surfaces is provided with a port, the port is equipped with a first sampling sleeve, and the TEM sample passes through all the inclined surfaces. The first sampling sleeve enters the cleaning chamber, wherein at least a pair of adjacent inclined surfaces have an included angle.

For the above device, in a possible implementation manner, the cleaning chamber is provided with an observation window in the direction facing the operator, and two sides of the observation window are respectively provided with an inclined surface, wherein the two inclined surfaces are directed toward the The operator's direction is inclined toward the middle of the viewing window.

For the above device, in a possible implementation manner, an openable window is provided above the cleaning chamber, so that the operation of putting into the cleaning chamber is completed by opening the window.

For the above device, in a possible embodiment, the vacuum storage module includes a storage chamber, the storage chamber includes at least one storage station, and a storage chamber is formed in the storage station and is connected with a second sample injection A sleeve, a sample rod or a carrying assembly enters the storage chamber through the second sampling sleeve, wherein the valve assembly includes at least one second valve corresponding to the storage station, and the second valve is set between the vacuum pump group and the corresponding storage station, so that the vacuum pump group is communicated with the corresponding storage station under the condition that the second valve is opened, so that the storage cavity of the storage station is connected. Vacuum extraction.

For the above device, in a possible embodiment, the carrying assembly includes a rod body, and a blocking part and a carrying part respectively provided at the first end and the second end of the rod body, and the carrying assembly can follow the direction from the rod body. The blocking part extends into the storage station from the direction of the carrying part, and in the fully extended state, the blocking part and the storage station are sealed and connected; wherein, the carrying part includes a base body, A placement unit is provided on the base, and the placement unit includes at least one placement location, each of which is capable of holding at least one TEM sample therein.

For the above device, in a possible implementation manner, the carrying portion is detachably disposed on the second end of the rod body.

For the above device, in a possible implementation manner, the plasma generator is provided with at least one external gas path for supplying the process gas, wherein the valve assembly includes at least one external gas path corresponding to the external gas path a third valve, the third valve is arranged between the vacuum pump group and the corresponding external air circuit so as to make the vacuum pump group and the corresponding external air circuit in the situation that the third valve is open communication to supply process gas into the cavity of the plasma generator.

For the above device, in a possible embodiment, the vacuum pump set includes a diaphragm pump and a molecular pump connected to each other, and the molecular pump can communicate with the plasma cleaning module and/or the vacuum storage module.

technical effect

(1) The device of the present invention can realize two kinds of pretreatments: plasma cleaning of TEM samples and vacuum storage of TEM samples and sample rods. Specifically, the plasma cleaning module can realize the cleaning of hydrocarbon contaminants and organic substances on the surface of the TEM sample, and the vacuum storage module can realize the drying and Clean preservation. Due to the shared vacuum pump group, not only the work efficiency is high, but also the parts and costs are greatly saved. Moreover, the working frequency of the same vacuum pump group is fixed, which avoids excessive mechanical vibration interference generated by different independent pretreatment equipment during the pretreatment of TEM samples and sample rods. Since the device of the present invention can independently implement two preprocessing functions, if it is necessary to connect the two preprocessing, the device of the present invention omits the need to independently process the two preprocessing functions in different equipment. It is necessary to transfer the steps, so as to effectively avoid the risk of TEM samples that may exist due to the need to transfer, such as falling during the transfer process.

(2) By adding an openable window (such as a quartz window) in the cleaning chamber, the device can meet the cleaning needs of TEM samples in more situations. By arranging inclined planes on both sides of the observation window, the plasma-cleaned sample can be located in the middle of the cleaning chamber, and the hand-held ends of the sample rods outside the first sampling sleeve are distributed in a figure-eight shape, so the hand-held ends of the two sample rods The ends do not collide.

(3) The storage station can not only realize the storage of the sample holder, but also can meet the requirement of vacuum storage of multiple TEM samples at one time by configuring the mounting components for the storage station. The mounting part of the mounting assembly is detachably provided on the rod body. It is possible to seek more diversified use of the ability of the mounting components to mount samples. For example, a variety of mounting parts of different specifications can be manufactured. When facing different mounting requirements, only the mounting parts can be replaced. In the case of needing to perform experiments on samples, remove the samples to be tested from the mounting assembly, and then mount the samples on the standard sample rods. The samples can be placed in the sample chambers of the experimental equipment through the cooperation of the sample rods with the experimental equipment. .

Description of drawings

The present utility model will be described below with reference to the accompanying drawings and in combination with the fact that the valves (the first, the second, and the third) are all solenoid valves and the TEM sample is a TEM sample bonded to a metal carrier mesh. In the attached picture:

Fig. 1 shows the working principle diagram of TEM;

FIG. 2 shows a schematic front view of an integrated device for preprocessing a transmission electron microscope sample and a sample rod according to the first embodiment of the present invention;

3 shows a schematic top view of the integrated device for pretreatment of a transmission electron microscope sample and a sample rod according to the first embodiment of the present invention, wherein, in the top view, the control module on the upper layer and the support plate and support rod on which the control module is installed are for perspective processing;

4 shows a schematic structural diagram of a cleaning chamber of an integrated device for pretreatment of a transmission electron microscope sample and a sample rod according to the first embodiment of the present invention;

5 shows a schematic structural diagram of a control module in an integrated device for preprocessing a transmission electron microscope sample and a sample rod according to the first embodiment of the present invention;

FIG. 6 shows a schematic structural diagram of the mounted components in the integrated device for the pretreatment of the transmission electron microscope sample and the sample rod according to the first embodiment of the present invention;

Fig. 7 shows the structural schematic diagram of the spring pressing piece;

FIG. 8 shows a schematic structural diagram of the mounting part in FIG. 6 when the spring pressing piece in FIG. 7 is installed;

Fig. 9 shows the assembly schematic diagram of the integrated device for the pretreatment of the transmission electron microscope sample and the sample rod according to the second embodiment of the present invention; and

FIG. 10 shows a schematic assembly diagram of an integrated device for pretreatment of a transmission electron microscope sample and a sample rod according to the third embodiment of the present invention.

List of reference numbers:

1. TEM; 11. Electron gun; 12. Condenser lens; 13. Sample room; 14. Objective lens; 15. Intermediate mirror; 16. Projection mirror; 17. Fluorescent screen; support plate; 23, support rod; 31, radio frequency power supply; 32, plasma generator; 321, port; 33, cleaning chamber; 331, observation window; 332, inclined plane; 3321, port; 333, first sampling sleeve 34, mass flow meter; 35, quartz window; 36, composite vacuum gauge; 361, port; 41, storage station; 42, second sampling sleeve; 43, sample rod; Regulation; 5, control module; 51, console; 52, countertop; 53, display screen; 54, alarm; 55, indicator light; 56, switch; 61, diaphragm pump; 62, molecular pump; 631, the first electromagnetic Valve; 632, second solenoid valve; 64, three-way valve; 7, carrying components; 71, rod body; 72, blocking part; 73, carrying part; 731, rounded rectangular sheet; 732, hole; 733, groove; 734, TEM sample; 735, hole; 736; logo; 8, spring clip; 81, first part; 811, hole; 82, second part; 83, third part; 84, screw.

Detailed ways

Various exemplary embodiments, features and aspects of the present invention are described in detail below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention, and are not intended to limit the protection scope of the present invention. Although this embodiment is described by taking the TEM sample as the TEM sample mounted on the metal mesh as an example, obviously, the sample can also be a directly prepared TEM sample in a non-mounted form.

It should be noted that in the description of the present invention, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner" and "outer" Terms such as the directions or positional relationships indicated are based on the directions or positional relationships shown in the drawings, which are for ease of description only, and do not indicate or imply that the device or element must have a particular orientation, be configured in a particular orientation, and operation, so it cannot be construed as a limitation to the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed to indicate or imply relative importance.

Furthermore, the same reference numerals in the figures denote elements that have the same or similar functions. While various aspects of the embodiments are shown in the drawings, the drawings are not necessarily drawn to scale unless otherwise indicated. Furthermore, any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.

In addition, in order to better illustrate the present invention, numerous specific details are given in the following detailed description. It should be understood by those skilled in the art that the present invention may be practiced without certain specific details. In some instances, methods and means well known to those skilled in the art have not been described in detail so as to highlight the gist of the present invention.

Example 1

Referring to FIGS. 2 to 4 , FIG. 2 shows a schematic front view of an integrated device for pretreatment of a transmission electron microscope sample and a sample rod according to the first embodiment of the present invention, and FIG. 3 shows the first embodiment of the present invention. Figure 4 is a schematic top view of the integrated device for the pretreatment of the transmission electron microscope sample and the sample rod, and FIG. 4 shows a schematic structural diagram of the cleaning cavity in the integrated device for the pretreatment of the transmission electron microscope sample and the sample rod according to the first embodiment of the present invention. . As shown in Fig. 2 to Fig. 4 , the device includes a stand, a plasma cleaning module for realizing plasma cleaning of TEM samples and a vacuum storage module for realizing vacuum storage of TEM samples and sample rods, and a plasma cleaning module and a vacuum set on the stand. The storage modules share a set of vacuum pumps capable of vacuum extraction/breaking. During the pretreatment of plasma cleaning and vacuum storage for TEM samples and sample rods, the control module is mainly used to control the vacuum pump group to perform vacuum extraction/removal of the plasma cleaning module and the vacuum storage module, so that the current TEM samples are cleaned and stored. The pretreatment is plasma cleaning or vacuum storage and other related electronic control operations. specifically:

The plasma cleaning module mainly includes a radio frequency power supply 31, a plasma generator 32 and a cleaning chamber 33. A cleaning chamber is formed inside the cleaning chamber. The oscillating field generated by the radio frequency power supply excites the process gas in the plasma generator, thereby providing sufficient cleaning chamber. Amounts of plasma and O radicals, plasma and O radicals can be used to plasma clean the samples in the cleaning chamber. According to the orientation in FIG. 3 , a mass flow meter 34 is arranged on the left side of the plasma generator, and an external gas path (not shown) for providing process gas is matched with the mass flow meter. For example, the mass flow meter is arranged in the external gas path Between the plasma gas generator and the plasma gas generator, the control module 5 controls the flow rate of the process gas from the external gas path leading to the cavity of the plasma generator according to the detection result of the mass flow meter. For example, the process gas may generally include Ar, O ₂ and H ₂ , preferably, a mixed gas of Ar and O ₂ or a mixed gas of H ₂ and O ₂ is used as the combined process gas.

Taking the plasma cleaning of the TEM sample placed on the sample holder as an example, for example, the process gas includes two kinds of Ar and O ₂ , and the two gases respectively lead to the cavity of the plasma generator through two external gas passages. , the two external gas circuits are respectively equipped with two mass flow meters, so that the control module can control the supply ratio of the two gases according to the detection results of the flow meters. After the two gases are mixed, they enter the cavity of the plasma generator to gradually increase the air pressure. The radio frequency power supply is activated to generate an oscillating field, and the process gas in the cavity is excited to generate a glow discharge to form Ar ⁺ plasma and active O radicals, Ar ⁺ plasma The bulk and active O radicals further enter the cleaning chamber of the cleaning chamber to act on the TEM sample in the cleaning chamber. Specifically, the active O radicals chemically react with the hydrocarbons on the surface of the TEM sample to generate CO, CO ₂ and H ₂ O (wherein the products may include one or both of CO and CO ₂ ) and are pumped by the vacuum pump The group is withdrawn from the cleaning chamber. Ar ⁺ removes C _x H _y from the surface of the TEM sample by means of physical collision. Finally, the cleaning of hydrocarbon contaminants and organics on the surface of TEM samples was achieved through the cooperation of physical and chemical effects.

Taking the plasma cleaning of the TEM carbon support film used to prepare the powder sample as an example, for example, the process gas only includes _O2 , open the quartz window at the top of the cleaning chamber, and put the carbon support film carrier mesh into the cleaning chamber When the process gas is passed through, O radicals can attach to the surface of the carbon film to achieve hydrophilic treatment. Afterwards, the powdered TEM sample is mixed with water or alcohol to form a suspension, which is dropped on the carbon film to form a TEM sample containing a carbon support film that can be directly subjected to TEM experiments. According to the orientation in FIG. 4 , an observation window 331 is provided in front of the cleaning chamber 33 . The observation window is mainly used to observe the glow discharge during the plasma cleaning process. The front of the cleaning chamber 33 has symmetrical positions on both sides of the observation window 331 . The inclined surfaces 332, each of the inclined surfaces 332 is provided with a port 3321, and the port is used to realize plasma cleaning of the sample rod 43 carrying the TEM sample in the cleaning chamber. Specifically, the port 3321 is equipped with a horizontally disposed first sampling sleeve 333 inclined from the outside to the inside, and the two first sampling sleeves are symmetrically distributed on both sides of the observation window and between the two first sampling sleeves Form an included angle of about 45°. In this way, it can be ensured that after the two sample rods enter the cleaning chamber through the corresponding first sampling sleeve-port respectively, the samples on the sample rods are located in the middle of the cleaning chamber, so that the cleaning efficiency is the highest, and the sample rods are located in the first Due to the figure-eight distribution of the hand-held end on the outside of the sampling sleeve, there is no collision. It can be understood that the inclined surface 332 may include a plurality of inclined surfaces, and the inclined surface may be set on one side or both sides of the observation window 331. The angle between the adjacent inclined surfaces may also be set flexibly. Those skilled in the art can flexibly choose according to the actual situation. As long as it is ensured that such an arrangement makes the operation more convenient and the advantages of the non-interference of multiple sample rods are clearly manifested. For example, two inclined surfaces 332 may be provided on both sides of the observation window 331, and an obtuse angle may be formed between the two inclined surfaces on the same side. different. The left side of the cleaning chamber 33 is provided with a port 361 for connecting the composite vacuum gauge 36, wherein the composite vacuum gauge is used to realize high vacuum measurement of the cleaning chamber. The rear of the cleaning chamber 33 is provided with a port 321 to which the plasma generator 32 is connected. The top of the cleaning chamber 33 is provided with an openable window, and the window is preferably a quartz window 35. When the quartz window is opened, a plurality of TEM samples (such as the TEM carbon support film or the TEM sample itself) can be placed from top to bottom. into the cleaning chamber, so as to ensure that the device can cope with large-scale situations such as cleaning more samples at one time or cleaning large samples.

Preferably, the radio frequency power supply of the plasma generator is powered by an AC power supply, the input voltage of the AC power supply is 220V, and the cleaning power in the cleaning process is 0-60W. Exemplarily, if it is used to clean the sample for hydrocarbon contaminants, the cleaning power is set to be ≥10W, and if it is used to perform hydrophilic treatment on the carbon support membrane, the cleaning power is set to be less than or equal to 5W.

The vacuum storage module includes a storage chamber arranged on the rack, and the storage chamber contains five storage stations 41 that are arranged in parallel and approximately in a square shape, and each storage station is formed with a storage chamber and connected with a second sampling sleeve 42 , after the sample rod 43 penetrates the second sampling sleeve, the head carrying the TEM sample is located in the storage cavity. The storage station is equipped with a resistance vacuum gauge 45 for making low vacuum measurements. The five storage stations may store the TEM sample rod and the TEM sample in the same way or differently.

In a possible implementation manner, among the 5 storage stations arranged in parallel, the 2 storage stations distributed on the left and right sides are mainly used for vacuum storage of the TEM sample rods that are matched and connected to the TEM. In this way, when a TEM experiment is required, the sample can be loaded on the sample holder 43 taken out from the storage station 41 . Of course, the TEM sample can also be mounted on the sample holder. In this way, the TEM sample can be stored at the same time through the cooperation of the sample holder 43 and the storage station 41 . If it is necessary to perform TEM experiments on the TEM sample, it can be directly taken out from the storage station. The structure of the sample rod and the manner in which the sample rod carries the sample are well known and will not be repeated here. The storage station in the middle is used for the simultaneous vacuum storage of multiple TEM samples using the modified piggyback assembly. Specifically, the following onboard components are used to store the samples:

Referring to FIGS. 6 to 8 , FIG. 6 shows the structural schematic diagram of the mounted components in the integrated device for the pretreatment of the transmission electron microscope sample and the sample rod according to the first embodiment of the present invention, and FIG. 7 shows the structural schematic diagram of the spring pressing piece. , FIG. 8 shows a schematic structural diagram of the mounting part in FIG. 6 when the spring pressing piece in FIG. 7 is installed. As shown in FIG. 6 to FIG. 8 and according to the orientation in FIG. 6 , the mounting assembly 7 mainly includes a rod body 71 , a blocking part 72 and a mounting part 73 respectively provided at the left and right ends of the rod body, and a plurality of TEM samples 734 are mounted on the same After one loading assembly, the loading assembly is pushed into the storage station from left to right, and in the assembled state, the sealing connection is achieved through the cooperation of the blocking portion 72 and the aforementioned second sampling sleeve 42 . When the TEM sample needs to be tested, the loading assembly 7 is first pulled out from the storage station 41, the TEM sample 734 to be tested is selected from the plurality of TEM samples and removed from the loading part 73, and then the TEM sample 734 to be tested is selected from the plurality of TEM samples. The TEM sample to be tested can be re-mounted on the sample holder 43 configured by the TEM, for example, the sample holder is the sample holder stored in the remaining four storage stations. The carrying portion 73 includes a base body with a plate-like structure and a plurality of placement positions on the base body, each placement position can place a TEM sample, and the left side of the base body is detachably fixed to the right end of the rod body.

In a possible implementation manner, the base body is a rectangular sheet with rounded corners formed at the top corners (hereinafter referred to as rounded rectangular sheet), and the left side of the rounded rectangular sheet 731 and the right side of the rod body 71 are provided with mounting holes 735 , the rounded rectangular sheet 731 is detachably fixed on the right end of the rod body 71 by means of fasteners (such as screws, etc.) in cooperation with the two mounting holes 735 . With this arrangement, the mounting assembly 7 can have more diverse mounting capabilities by replacing the rounded rectangular pieces 731 . For example, the mounting parts of various specifications can be pre-arranged, and the mounting capacity of the mounting components can be adjusted by replacing only the mounting parts according to the type and number of samples. In addition, such an improvement can be made further by adding a corresponding connecting structure on the carrying part. As long as the form and standard of the connecting structure are formulated in advance, the expansion of the carrying part can be sought according to the actual situation. Specifically, the mounting portion 73 serving as a basic function remains connected to the second end of the rod body 71 , and the mounting portion serving as an extended function only needs to be directly or indirectly connected to the mounting portion serving as a basic function by means of a connecting structure. In this way, the vacuum storage capacity of different types of samples can be flexibly adjusted by flexibly adjusting the capacity of the carrying part. Alternatively, more structures that can realize matching may be reserved at the second end of the rod body.

The rounded rectangular sheet 731 is provided with a plurality of grooves 733 serving as placement positions. Specifically, the 6 grooves are neatly arranged in two upper and lower rows, and each row includes 3 grooves that are equally spaced, and each groove can accommodate one TEM samples. Therefore, the mounting portion 73 can mount six TEM samples. The way to fix the TEM sample 734 on the rounded rectangular sheet 731 may be, for example, a hole 732 is provided on the rounded rectangular sheet at a position corresponding to each slot 733, specifically, each slot is arranged in parallel at the horizontal left position There is one hole, and each pair of corresponding holes and grooves corresponds to a set position, and each set position is provided with a spring pressing piece 8 to realize the fixation of the TEM sample 734 . In addition, the area on the left side of the hole 32 on the rounded rectangular sheet 731 is provided with a mark 736 corresponding to the sample, such as a mark with a number or the like.

In a possible embodiment, as shown in FIGS. 7 and 8 and according to the orientation in FIG. 7 , the spring pressing piece 8 includes a first part 81 from left to right, a second part 82 and a part located therebetween. The third part 83, the first part and the second part are parallel to each other and arranged in a horizontal direction, and the third part is a structure inclined downward from left to right. The first part 81 is provided with a hole 811 that can be matched with the hole on the rounded rectangular sheet 731 , and the screw 84 as a fastener can pass through the hole 811 on the first part 81 and correspond to the rounded rectangular sheet 731 . The holes 732 of each seating position are matched, so that the spring pressing piece 8 is screwed and fixed to the rounded rectangular sheet 731. At this time, the second part 82 covers the opening of the groove 733 of the seating position of the rounded rectangular sheet and abuts against the TEM sample. 734 to hold the TEM sample in the groove. It can be understood that the spring pressing piece as the connection structure is only an exemplary description. Obviously, those skilled in the art can use other structural forms according to the actual situation, or use any other reasonable way to replace the connection member, only the It is necessary to ensure that the TEM sample can be fixed in the groove and that this fixing constraint can be released.

In a specific embodiment, the width (upper-down direction) of the rounded rectangular sheet 731 does not exceed 15 mm (preferably 15 mm), and the thickness (inner-outer direction) is 1-2 mm (preferably 2 mm); the rounded rectangular sheet 731 Use metal materials (such as aluminum alloy or stainless steel). The thickness of the spring pressing piece (up-down direction) does not exceed 100μm, the width (inner-outer direction) is 3mm, and the length (left-right direction) is 10mm, and the material is copper alloy.

In application, firstly, the prepared lamellar TEM sample is bonded to the TEM metal carrier, and then the TEM metal carrier is placed in the groove, and then the spring pressing piece is fixed on the rounded rectangular piece, which can be passed through the spring pressing piece. The function of the second part is to hold the TEM metal grid in the groove. Afterwards, the loading assembly with the rounded rectangular sheet of multiple TEM metal carrier meshes is pushed into the storage station until the sealing part of the loading assembly is sealed with the storage station.

It can be understood that a person skilled in the art can flexibly set the carrying portion, the specific form of the placement position, and the distribution of the placement position on the carrying portion, etc. according to actual needs. For example, the vacuum storage device can be equipped with multiple loading parts of different specifications, and according to the type and number of samples, only the loading part can be replaced to meet the storage requirements.

Since the above-mentioned mounting assembly 7 is only for vacuum storage of TEM samples, the blocking part can be designed in a simpler status, for example, the blocking part can be designed in a compact plug shape according to the actual situation. In contrast, the sample rod 43 is used as a standard part, the radial dimension of the hand-held end is about 8 cm, and the diameter of the plug-shaped blocking part is only a plug with a diameter of 2 cm (hereinafter referred to as plugging), in addition, it can also be 5 storage stations. The second sampling sleeve 42 of the second sample introduction sleeve 42 is equipped with a plug 44. When any storage station is not in use, it can be blocked by the configured plug, so as to achieve simple functions such as preventing impurities and dust. It can be seen that, compared with the direct storage of the sample rod, the improved mounting assembly has a smaller size, and on the premise of satisfying the use performance, there can be a smaller distance between adjacent storage stations, so as to achieve better performance. More compact design. As in this embodiment, the horizontal distance between the two storage positions 41 for storing sample rods on both sides must be greater than 8 cm, and the distance between the storage position in the middle and the adjacent storage positions for storing sample rods The horizontal distance between them only needs to be greater than 5cm.

The vacuum pump set is mainly used to realize the vacuum extraction/removal requirements of the cleaning chamber in the cleaning chamber 33 in the plasma cleaning module and the storage chamber in the storage station 41 in the vacuum storage module. In this embodiment, the vacuum pump set includes a fore pump and a secondary pump, the fore pump is preferably a diaphragm pump 61, the secondary pump is preferably a molecular pump 62, the diaphragm pump is connected to the molecular pump, and the molecular pump is connected to the cleaning chamber through a pipeline It is respectively connected with the storage chamber to realize plasma cleaning of TEM samples, sample holder (with or without TEM samples) and vacuum storage of multiple TEM samples mounted on the aforementioned mounting components. For example, the molecular pump 62, the cleaning chamber and the storage chamber are connected by a three-way valve 64 and related connecting parts, such as bellows, flanges and related pipelines. In the process of plasma cleaning of TEM samples, the external gas circuit supplies process gas to the cavity of the plasma generator 32 by means of the vacuum pressure formed by the diaphragm pump and the molecular pump. For example, the molecules can be flexibly selected according to the number of external gas circuits. The connection between the pump and the external air circuit. For example, a multi-port valve can be used to connect the molecular pump to the cleaning chamber, the storage chamber and each external air circuit respectively.

It can be understood that those skilled in the art can select the number of stages of the vacuum pump set and the types and specifications of the pumps at each stage according to the actual situation, as long as it can ensure that the pump set can realize the vacuum extraction/removal of the cleaning chamber and the storage chamber and the supply of the plasma. The function of the generator to supply/block the process gas is sufficient. The connection mode between the vacuum pump unit and the downstream cleaning chamber, storage chamber and external air circuit can also be selected in a suitable connection form. branch, etc.

Exemplarily, the vacuum pump set is configured with a solenoid valve set, the solenoid valve set includes a first solenoid valve 631, a second solenoid valve 632, a third solenoid valve (not shown) and a purge valve (not shown), wherein the first solenoid valve 631 A solenoid valve 631 is arranged between the molecular pump 62 and the cleaning chamber 33, and the control module 5 realizes the vacuum extraction/breaking of the cleaning chamber by controlling the opening and closing of the first solenoid valve 631 and by means of the diaphragm pump and the molecular pump. Each storage station is equipped with a second solenoid valve, and the control module realizes the vacuum extraction/breaking of the storage cavity of each storage station 41 by controlling the opening and closing of the second solenoid valve 632 and by means of a diaphragm pump and a molecular pump. Each external air circuit is equipped with a third solenoid valve, and the third solenoid valve is located between the plasma generator and the corresponding external air circuit. The control module controls the third electromagnetic valve according to the detection result of the mass flowmeter on the corresponding external air circuit. The valve is opened and closed and the corresponding process gas is supplied/blocked by means of a two-stage pump. The air release valve is provided in the cleaning chamber and communicates with the ambient air when the cleaning chamber is opened so as to realize the vacuum breaking.

FIG. 5 shows a schematic structural diagram of a control module in an integrated device for preprocessing a transmission electron microscope sample and a sample rod according to the first embodiment of the present invention. As shown in FIGS. 2 and 5 and according to the orientation in FIG. 5 , for example, the control module 5 includes a console 51 arranged on the platform 1, and a circuit board for realizing the aforementioned control functions is arranged on the console. A display table is arranged on the side, and the display table has a downwardly inclined table 52. The table is provided with a display screen 53 that allows users to perform interactive operations and can display relevant information, an alarm 54 for giving sound and light reminders, and a standby indication. Light 55 and switch 56 for starting/stopping the device.

2 and 3, the stand 2 includes a base 21, the radio frequency power supply 31 is fixed on the base 21, and the five parallel storage stations 41 are located directly above the radio frequency power supply. Specifically, a support plate is provided above the radio frequency power supply 31. 22. The 5 parallel storage stations are all fixed on the support plate, and the support plate is supported and fixed by a plurality of support rods 23 fixed on the base 21. For example, in this embodiment, the number of support rods is 4, which are respectively arranged on the base. and the four corners of the support plate. The 5 storage stations are on the same level and below the 2 first sampling sleeves of the cleaning chamber in the plasma cleaning module, and the 5 storage stations 41 and the 2 first sampling sleeves 333 of the cleaning chamber 33 are located directly on the front side of the unit. Such an arrangement can achieve the convenience of the device during operation, and make the sample holder carrying the TEM sample not easily interfered during preprocessing, and the operator can easily obtain any sample holder, thus ensuring that the sample holder has the higher security.

Based on the above structure, the method for plasma cleaning and vacuum storage for the same sample holder with the sample is as follows:

First, the TEM sample 734 on the sample holder 43 is plasma cleaned. The specific steps are as follows: turn on the switch, turn on the air release valve and the first solenoid valve 631 in turn, after the vacuum in the cleaning chamber is broken, remove the plug 44 on the first sampling sleeve 333 directly in front of the cleaning chamber 33, and then load the The sample rod 43 with the TEM sample is inserted into the first sampling sleeve 333; the air release valve is closed, the vacuum pump set is started, and the cleaning chamber is pre-evacuated by the diaphragm pump 61 and the molecular pump 62. In order to further improve the vacuum extraction efficiency, the storage Each of the second solenoid valves 632 configured at the station 41 is closed. The composite vacuum gauge 36 detects the vacuum degree of the cleaning chamber. After the vacuum degree of the cleaning chamber reaches the standard (for example, it reaches 10 ^-5 Torr), the third solenoid valve corresponding to the external air circuit is opened, and the control module 5 is based on the detection of the mass flow meter 34 . As a result, a predetermined type of process gas is delivered to the cavity of the plasma generator 32 through the corresponding external gas path. In this embodiment, two process gases, Ar and O ₂ are selected to be delivered to the cleaning cavity, and the radio frequency power supply 31 is activated to generate an oscillating field to excite the Ar and O ₂ in the cavity generate glow discharge to form plasma and active O radicals and further pass into the cleaning cavity to clean the hydrocarbon contaminants and organic substances on the surface of the TEM sample 734 . After cleaning, interrupt the external air circuit and turn off the RF power supply.

Next, vacuum storage of the sample holder 43 is performed. The specific steps are as follows: after the plasma cleaning is completed, insert the head of the sample rod 43 into the storage cavity of the storage station 41 in the vacuum storage module along the second sampling sleeve 42, open the corresponding second solenoid valve 632, and activate the diaphragm The pump 61 and the molecular pump 62 continuously evacuate the storage chamber until the vacuum reaches the standard (for example, the same level as that of the cleaning chamber); maintain the vacuum degree of the storage chamber, so that the sample holder 43 and the TEM sample 734 mounted on the sample holder are both evacuated. Continuous storage in a vacuum environment.

The above embodiment is described by taking the TEM sample 734 mounted on the sample holder 43 as an example. Obviously, the TEM sample 734 can also be mounted on the aforementioned mounting assembly 7 . Corresponding to such a TEM sample, the plasma cleaning of the TEM sample is realized by inserting the sample rod into the cleaning cavity when the TEM sample is plasma cleaned. Obviously, for a sample such as a TEM carbon support film, the carbon support film carrier mesh should be put into the cleaning chamber first by opening the quartz window.

The above embodiment is the operation steps of sequentially performing plasma cleaning and vacuum storage for the same TEM sample. Of course, the device of the present invention can also meet the needs of other pretreatments, such as: setting the storage chamber to have an inserted sample rod or Onboard components, which can also be individually vacuum-stored. The sample holder can carry or not carry the TEM sample. If the TEM sample is not carried, the sample holder is mainly stored in vacuum. If the TEM sample is carried, the sample holder and the TEM sample are stored in vacuum together.

It can be understood that under the premise that the structures of each component are basically the same, and under the condition that the functions can be realized without interference, those skilled in the art can flexibly adjust the setting orientation of each component according to the actual situation, or adjust the setting of each component. The structure is fine-tuned. like:

Example 2

Referring to FIG. 9 , FIG. 9 shows a schematic assembly diagram of an integrated device for preprocessing a transmission electron microscope sample and a sample rod according to the second embodiment of the present invention. As shown in Figure 9, the two first sampling sleeves of the plasma cleaning module are coplanar and have an included angle from outside to inside; the five second sampling sleeves of the vacuum storage module are parallel and coplanar, The planes formed by the (first and second) sampling sleeves are arranged parallel to each other up and down, and all sampling sleeves are generally located on the same side of the device, such as the side facing the operator, which is easy to operate and improve Safety of the sample holder. The five storage stations 41 of the vacuum storage module corresponding to the five second sampling sleeves are fixed on the base 21 of the gantry, the lower support plate 22 is supported and fixed by the support rods 23 fixed on the base 21, and the radio frequency power supply 31 is located in the vacuum Just above the five storage stations 41 of the storage module, the two are separated by the low-level support plate 22, the radio frequency power supply 31 is fixed on the upper surface of the low-level support plate 22, and a high-level power supply 31 is provided above the radio frequency power supply 31. The support plate 22 , the high-level support plate 22 is fixed by the support rods 23 from the base 21 , and the control module 5 is fixed on the upper surface of the high-level support plate 22 , that is, directly above the RF power source 31 . The positions of other components are basically unchanged, as shown in the figure, the cleaning chamber 33 and the molecular pump 62 are both arranged on the right side and the two are connected through a three-way valve 64.

Example 3

Referring to FIG. 10 , FIG. 10 shows an assembly schematic diagram of an integrated device for preprocessing a transmission electron microscope sample and a sample rod according to the third embodiment of the present invention. As shown in Figure 10, the vacuum storage module is located above the plasma cleaning module, and the vacuum pump group is located below, such as the molecular pump 62 is arranged on the base 21 of the stand. The vacuum pump group and the plasma cleaning module are communicated through corresponding pipelines, and the vacuum storage module is directly communicated with the cleaning chamber in the plasma cleaning module, so as to communicate with the vacuum pump group through the cleaning chamber in the plasma cleaning module. Specifically, in the plasma cleaning module, the plasma generator 32 is located on the left side of the cleaning chamber 33, the two first sampling sleeves of the cleaning chamber 33 are coplanar and have an angle from outside to inside, the vacuum storage module The five second sampling sleeves are parallel and coplanar, and the planes respectively formed by the (first and second) sampling sleeves are parallel to each other up and down. The five storage stations 41 of the vacuum storage module corresponding to the five second sampling sleeves are located on the topmost layer of the device and are placed at the topmost position outside the rack. The advantage of this setup is that during vacuum storage of the TEM sample and sample holder, the sample on the sample holder can be viewed from the external storage chamber glass screen. In addition, based on such an installation orientation, a drawer-type sample stage that can be pushed and pulled can be added to the right side of the cleaning chamber 33, so as to realize the cleaning of multiple TEM samples or bulk samples, etc., so as to achieve larger Sample processing scale.

It should be noted that although the above technical solutions are introduced as examples, those skilled in the art can understand that the present invention should not be limited to this, and users can flexibly set vacuum systems, plasma cleaning modules and samples according to actual application scenarios and other situations. Technical parameters of the rod storage module, etc.

So far, the technical solutions of the present invention have been described with reference to the preferred embodiments shown in the accompanying drawings, but those skilled in the art should readily understand that the protection scope of the present invention is obviously not limited to these specific embodiments. On the premise of not departing from the principles of the present invention, those skilled in the art can make equivalent changes or replacements to the relevant technical features, and the technical solutions after these changes or replacements will fall within the protection scope of the present invention.

Claims (10)

1. An integrated transmission electron microscope sample and sample rod pretreatment apparatus, comprising:

the plasma cleaning module is used for carrying out plasma cleaning on the TEM sample;

the vacuum storage module is used for carrying out vacuum storage on the TEM sample and/or the sample rod;

a vacuum pump set capable of communicating with the plasma cleaning module and the vacuum storage module, respectively; and

a valve assembly including a plurality of valves, the vacuum pump set communicating with the plasma cleaning module and/or the vacuum storage module by switching an open/closed state of one or more of the plurality of valves.

2. The apparatus of claim 1, wherein the plasma cleaning module comprises a radio frequency power supply, a plasma generator and a cleaning chamber, a cleaning cavity is formed inside the cleaning chamber, an oscillating field generated by the radio frequency power supply excites a process gas entering the plasma generator to generate plasma, so as to clean the sample in the cleaning cavity,

wherein the valve assembly comprises a first valve which is arranged between the vacuum pump group and the cleaning chamber so as to communicate the vacuum pump group with the cleaning chamber under the condition that the first valve is opened to perform vacuum extraction on the cleaning cavity.

3. The apparatus of claim 2, wherein a plurality of ramps are provided on the wash chamber, each ramp having a port provided thereon, the port being fitted with a first sample sleeve through which TEM samples enter the wash chamber,

wherein, an included angle is formed between at least one pair of adjacent inclined surfaces.

4. A device according to claim 3, characterized in that the washing chamber is provided with a viewing window in a direction facing the operator, said viewing window being provided with a bevel on each side,

wherein the two inclined surfaces are inclined toward a middle of the observation window in a direction toward the operator.

5. The device according to claim 2, characterized in that an openable window is arranged above the washing chamber, so that the throwing operation into the washing chamber is completed by opening the window.

6. The apparatus according to any one of claims 1 to 5, wherein the vacuum storage module comprises a storage chamber comprising at least one storage station in which a storage chamber is formed and in which a second sample sleeve is connected, through which a sample rod or carrier assembly enters the storage chamber,

wherein the valve assembly comprises at least one second valve corresponding to the storage station, and the second valve is arranged between the vacuum pump group and the corresponding storage station so as to communicate the vacuum pump group with the corresponding storage station under the condition that the second valve is opened to perform vacuum extraction on the storage cavity of the storage station.

7. The apparatus of claim 6, wherein the carrying assembly comprises a rod body, and a blocking portion and a carrying portion respectively disposed at a first end and a second end of the rod body, the carrying assembly being extendable into the storage station in a direction from the blocking portion to the carrying portion, and wherein the carrying assembly is extendable into the storage station

In a fully extended state, the blocking part is in sealing connection with the storage station;

wherein the mounting portion comprises a base on which a mounting unit is provided, the mounting unit comprising at least one mounting location, each mounting location capable of holding at least one TEM sample therein.

8. The apparatus of claim 7, wherein the mounting portion is removably disposed at the second end of the rod.

9. The apparatus according to claim 2, wherein the plasma generator is provided with at least one external gas path for supplying the process gas,

wherein the valve assembly comprises at least one third valve corresponding to the external gas circuit, and the third valve is arranged between the vacuum pump set and the corresponding external gas circuit so as to communicate the vacuum pump set with the corresponding external gas circuit under the condition that the third valve is opened to supply the process gas into the cavity of the plasma generator.

10. The apparatus of claim 1, wherein the vacuum pump set comprises a diaphragm pump and a molecular pump connected to each other, the molecular pump being communicable with the plasma cleaning module and/or the vacuum storage module.

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