WO2022001107A1

WO2022001107A1 - System and method for self-driven vacuum transfer of sample

Info

Publication number: WO2022001107A1
Application number: PCT/CN2021/075265
Authority: WO
Inventors: 张小波; 常正凯; 闻益
Original assignee: 深圳市速普仪器有限公司
Priority date: 2020-06-30
Filing date: 2021-02-04
Publication date: 2022-01-06
Also published as: CN111731677A

Abstract

A system and method for vacuum transfer of a sample, the system for vacuum transfer of a sample comprising a vacuum box and a vacuum pump set (600), wherein the vacuum box comprises a box body (100), a self-driven sample ejection stage (200), a vacuum sealing valve body (300), a vacuum sealing valve air nozzle (400) and a sample holder (700); the self-driven ejection sample stage (200) is provided with a cover plate (210), a bracket member and an elastic member (260) which are connected in sequence; one end of the elastic member (260) is fixed inside the box body (100), and the other end thereof movably abuts against a support piece. When the elastic member (260) is in a compressed state, a cover plate (210) is in contact with the box body (100) and the cover plate (210) and the box body (100) together form a closed cavity (180), and the support piece is located in the cavity (180). When the elastic member (260) is in a free state, the sample holder (700) is located outside the box body (100). The vacuum sealing valve body (300) is in communication with the cavity (180) and the vacuum sealing valve air nozzle (400) respectively. The sample holder (700) is detachably arranged on the support piece, and the vacuum sealing valve air nozzle (400) is used for connecting the vacuum pump set (600).

Description

Self-propelled sample vacuum transfer system and method

CROSS-REFERENCE TO RELATED APPLICATIONS

This application claims the priority of the Chinese patent application with the application number 2020106103083 and the invention titled "Self-driven sample vacuum transfer system and method" filed with the China Patent Office on June 30, 2020, the entire contents of which are incorporated herein by reference Applying.

technical field

The present application relates to the field of sample transfer, in particular to a self-driven sample vacuum transfer system and method.

technical background

Glove boxes, scanning electron microscopes, and micro-nano-processing systems have been widely used in traditional materials, advanced new materials, semiconductor materials, nanomaterials, and catalytic materials. It realizes direct fine processing and high-resolution characterization of magnetic materials, low dielectric coefficient materials, biomedical materials, polymer composite materials and ceramic materials, and shows great potential in the fields of new materials, environment, energy and chemistry. However, in specific applications, some samples are at risk of contamination or oxidation by air or moisture during preparation, storage and transfer. To avoid contamination or oxidation of air or moisture-sensitive materials during preparation, storage and transfer, a dry protective atmosphere or vacuum environment is required throughout. The sample vacuum transfer system is undoubtedly the key technology to solve the problem. Existing sample vacuum transfer technologies generally use external or built-in electric drive devices, such as the commercial vacuum transfer device products of Kammrath-Weiss Company in Germany, etc., which are integrated with the vacuum system through motors, control devices, and guide devices to drive and control the vacuum. Opening and closing of the system cover.

Although the current electric-driven vacuum transfer device can realize the storage and transfer functions of sensitive samples, there are the following problems in the specific use process: (1) The electric-driven vacuum transfer device integrates components such as motors and guide devices. , generally large in size, for some compact SEMs, such as desktop SEMs, etc., cannot accommodate such a volume of vacuum transfer devices; (2) In order to realize electric drive and control, glove boxes, SEMs and micro-nano are required. The processing system provides corresponding electronic control interfaces for internal and external power connection, and involves the compatibility of interfaces of different specifications, which invisibly increases the complexity and cost of the system and raises the threshold for cross-platform transfer.

SUMMARY OF THE INVENTION

According to various embodiments of the present application, a self-propelled sample vacuum transfer system and method are provided.

A sample vacuum transfer system includes a vacuum box and a vacuum pump set. The vacuum box includes a box body, a self-driven ejecting sample stage, a vacuum sealing valve body, a vacuum sealing valve air nozzle and a sample holder. The self-driven ejection sample stage is provided with a cover plate, a bracket member and an elastic member which are connected in sequence. One end of the elastic member is fixed inside the box body, and the other end is movably abutted against the bracket member. The sample holder is detachably arranged on the support member. When the elastic member is in a compressed state, the cover plate is in contact with the box body, and the cover plate and the box body together form a closed cavity, and the bracket member is located in the cavity. The elastic member is in a free state, and the sample holder is located outside the box. The vacuum sealing valve body is respectively communicated with the chamber and the air nozzle of the vacuum sealing valve. The vacuum sealing valve air nozzle is used to connect the vacuum pump group.

The above self-driven sample vacuum transfer system is used for storage and transfer in the sample preparation process. It has the advantages of simple structure, cleverly utilizes the pressure formed by the vacuum environment, and can drive the sample by itself when the pressure difference between the internal and external gases reaches a certain condition. In order to carry out the next operation, it does not involve electric drive at all, which is beneficial to reduce its own volume beyond expectations, especially suitable for the use of compact sample processing equipment, compatible with most sample processing platforms such as sample preparation and characterization platforms , which solves the problem of high cost of sample pretreatment caused by the complex structure and low versatility of the existing related systems, thereby helping to improve the versatility of non-destructive cross-platform transfer of sensitive samples such as air or water vapor sensitive samples.

A sample vacuum transfer method, comprising providing the sample vacuum transfer system described in any one of the above; placing the sample in a sample holder; placing the sample holder on a bracket member of a self-driven ejection sample stage; The bracket piece is pushed into the chamber of the box body and the cover plate of the self-driven ejection sample stage is brought into contact with the box body to close the chamber; Evacuate; close the vacuum seal valve nozzle; and transfer the vacuum box as a whole to the target platform.

Description of drawings

FIG. 1 is a perspective view of a sample vacuum transfer system according to an embodiment.

FIG. 2 is a front view of the sample vacuum transfer system shown in FIG. 1 .

FIG. 3 is a cross-sectional view taken along line A-A in FIG. 2 .

FIG. 4 is a right side view of the system shown in FIG. 1 .

FIG. 5 is a perspective view of the self-driven ejection sample stage of the sample vacuum transfer system shown in FIG. 1 when it is opened.

FIG. 6 is a front view of the sample vacuum transfer system shown in FIG. 5 .

FIG. 7 is a cross-sectional view taken along line B-B in FIG. 6 .

FIG. 8 is a right side view of the system shown in FIG. 5 .

9 is a front view of a partial structure of a sample vacuum transfer device according to another embodiment.

FIG. 10 is a left side view of the device shown in FIG. 9 .

FIG. 11 is a perspective view of the device shown in FIG. 9 .

12 is a perspective view of a vacuum transfer apparatus according to another embodiment.

FIG. 13 is a front view of the vacuum transfer apparatus shown in FIG. 12 .

FIG. 14 is a top view of the vacuum transfer apparatus shown in FIG. 12 .

FIG. 15 is a perspective view of the self-driven ejection sample stage of the vacuum transfer device shown in FIG. 12 when it is opened.

FIG. 16 is a top view of the vacuum transfer apparatus shown in FIG. 15 .

detailed description

In order to make the above objects, features and advantages of the present application more clearly understood, the specific embodiments of the present application will be described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present application. Therefore, the present application is not limited by the specific embodiments disclosed below.

It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or an intervening element may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical", "horizontal", "left", "right" and similar expressions used in the specification of this application are for illustrative purposes only and do not represent the only embodiment.

Unless otherwise defined, all technical and scientific terms used in the specification of this application have the same meaning as commonly understood by one of ordinary skill in the technical field to which this application belongs. The terms used in the specification of the present application are for the purpose of describing specific embodiments only, and are not intended to limit the present application. As used in this specification, the term "and/or" includes any and all combinations of one or more of the associated listed items.

In one embodiment, as shown in FIG. 1, a self-propelled sample vacuum transfer system includes a vacuum box. Please refer to FIG. 2 and FIG. 3 together, the vacuum box includes a box body 100, a self-driven ejection sample stage 200, a vacuum sealing valve body 300, a vacuum sealing valve air nozzle 400 and a sample holder 700; the vacuum sealing valve body 300 is provided with a vacuum sealing The valve switch 500, the vacuum sealing valve air nozzle 400 has an on state and a closed state, the vacuum sealing valve body 300 is used to communicate with the vacuum pump group 600 through the vacuum sealing valve air nozzle 400 in the conductive state, and after the vacuum is pumped, the vacuum seal is closed. The self-driven sample vacuum transfer system can be transferred with the valve air nozzle 400 in a closed state. The vacuum sealing valve body 300 is fixed on the box body 100 by the fixing member 310 .

When the elastic member 260 is in a certain compressed state, the cover plate 210 is in contact with the box body 100, and the cover plate 210 and the box body 100 together form a closed cavity 180, and the bracket member is located at the In the chamber 180; in this embodiment, the box body 100 is provided with an upper box plate 110, a lower box plate 120, a bottom box plate 140 and a side box plate, an upper box plate 110, a lower box plate 120, a bottom box plate 140 and The side box plates are jointly enclosed and arranged so that part or all of the cavity 180 is formed inside the box body 100 , that is, part or all of the cavity 180 is arranged inside the box body 100 , and the bottom box plate 140 passes through the fixing device 150 and the upper box plate 110 respectively. and the lower box plate 120 are fixed. The box body 100 is also provided with an upper guide rail 160 and a lower guide rail 170. The vacuum sealing valve body 300 is respectively connected to the chamber 180 and the vacuum sealing valve air nozzle 400. The vacuum sealing valve air nozzle 400 is used to connect the vacuum pump set 600; the inside of the box body 100 A resisting member 130 is provided; in this embodiment, the resisting member 130 is fixedly disposed on the bottom box plate 140 .

The self-driven ejection stage 200 is provided with a cover plate 210 , a bracket member and an elastic member 260 which are connected in sequence. The cover plate 210 is in the shape of a flat plate, and the box body 100 is in the shape of a prism. The self-driven ejection stage 200 is further provided with a guide shaft 270 and a mounting portion 271 . The mounting portion 271 is fixed inside the box body 100 , one end of the guide shaft 270 is fixed on the abutting member 130 , and the other end is fixed on the mounting portion 271 and guides The shaft 270 is disposed through the bracket member, one end of the elastic member 260 is fixed on the abutting member 130, and the other end is movably abutted on the bracket member. The sample holder 700 is detachably arranged on the bracket member; the bracket member is provided with an upper bracket 240 connected in sequence , the inner bracket 250 and the lower bracket 230, the sample holder 700 is detachably arranged on the upper bracket 240; the upper bracket 240 is slidably arranged on the upper rail 160, and the lower bracket 230 is slidably arranged on the lower rail 170; The positioning portion 241 of the sample holder 700 is fixed under a certain force; the bracket member is further provided with an outer bracket 220, the upper bracket 240 and the lower bracket 230 are respectively connected with the outer bracket 220, and the outer bracket 220 is connected with the cover plate 210; A middle bracket 280 is also arranged between the outer bracket 220 and the inner bracket 250 , the upper bracket 240 and the lower bracket 230 are respectively connected with the middle bracket 280 , the guide shaft 270 is arranged through the inner bracket 250 , and the guide shaft 270 also passes through the middle bracket 280 set up. One end of the elastic member 260 is fixed on the resisting member 130, and the other end is movably abutted against the inner bracket 250; the elastic member 260 is a hollow member and the elastic member 260 is sleeved outside the guide shaft 270. Move along the guide shaft 270 . As shown in FIG. 3 and FIG. 4 , when the elastic member 260 is in a certain compressed state, the cover plate 210 is in contact with the box body 100 to close the cavity 180 and the bracket member is located in the cavity 180 .

As shown in FIG. 5 , when the elastic member 260 is in a free state, the sample holder 700 is located outside the box body 100 . Please refer to FIG. 6 and FIG. 7 together. The sample holder 700 includes a connected tray 710 and a fixed end 720. The tray 710 is used to carry the sample. The bracket is provided with a fixed groove corresponding to the fixed end 720. The fixed end 720 is detachable It is fixed in the fixing groove so that the tray 710 can be detachably arranged on the bracket. At this time, the mounting portion 271 abuts against the inner bracket 250 to restrict the elastic member 260 from further extending outward, and the sample holder 700 and its tray 710 are all located outside the box body 100 . Please also refer to FIG. 8 , the self-driven sample vacuum transfer system is further provided with a sealing gasket 800 on the box body 100 or the cover plate 210 . When the elastic member 260 is in a certain compressed state, the cover plate 210 is connected to the box body 100 through the sealing gasket 800 . contact to close the chamber 180 .

In order to better show the internal structure of the vacuum box, in one embodiment, as shown in FIG. 9 , FIG. 10 and FIG. 11 , the number of guide shafts 270 is two, and each guide shaft 270 is provided with a spring as an elastic The cover plate 210 fixes the upper bracket 240 and the outer bracket 220 through the fixing part 290 ; one end of the guide shaft 270 is fixed on the abutting member 130 , and the other end is fixed on the mounting part 271 , and the upper bracket 240 is fixed on the inner bracket 240 through the fixing part 290 . Bracket 250. The box body 100 is provided with a resisting member 130 on the bottom box plate 140 , one end of the elastic member 260 is fixed on the resisting member 130 , and the other end movably abuts against the mounting portion 271 , that is, the other end of the elastic member 260 abuts and mounts in a compressed state The mounting portion 271 may be in contact with the mounting portion 271 in a free state, or there may be a gap between the mounting portion 271 and the length of the guide shaft 270 and the elastic force of the elastic member 260 .

In one embodiment, as shown in FIGS. 12 , 13 and 14 , a self-driven sample vacuum transfer system includes a vacuum box 900 and a vacuum pump set 600 . When in use, the vacuum pump set 600 is connected to the vacuum box 900 through the pipe body, and when transferring the sample, only the vacuum box 900 needs to be transferred. 15 and 16, the vacuum box 900 includes a box body 100, a self-driving sample ejection stage 200, a vacuum sealing valve body 300, a vacuum sealing valve gas The nozzle 400 and the sample holder 700; the vacuum seal valve body 300 is provided with a vacuum seal valve switch 500, and the sample holder 700 is located outside the box body 100 at this time, so that the samples carried by the sample holder 700 can be processed automatically or manually. The vacuum seal valve switch 500 is used to make the vacuum seal valve body 300 and the chamber 180 be in a closed state or an open state when the vacuum seal valve air nozzle 400 is in a closed state.

In one of the embodiments, the present application also provides a self-driven sample vacuum transfer method, the method comprising providing the sample vacuum transfer system of any of the above embodiments; placing the sample in the sample holder; placing the sample in the sample holder On the bracket of the self-driven ejection stage; push the bracket of the self-driven ejection stage into the chamber of the cassette body and make the cover plate of the self-driven ejection stage come into contact with the cassette body to close the chamber; by vacuum sealing The valve air nozzle evacuates the vacuum sealing valve body and the connected chamber; closes the vacuum sealing valve air nozzle; the body transfers the vacuum box.

In one embodiment, transferring the vacuum box as a whole includes: transferring the vacuum box as a whole to the target platform; and after transferring the vacuum box as a whole, the self-driven sample vacuum transfer method further includes the step of: vacuuming on the target platform to the self-propelled sample platform. The elastic member that drives the ejection stage ejects the support member and keeps the sample holder outside the box. In this design, only the vacuum box is transferred, which has the advantage of small size. And the whole process is cleverly controlled by vacuum pressure and elastic force, without electric drive.

The following takes lithium-ion battery materials as an example to further describe the specific applications of the embodiments of the present application. It can be understood that the present application is also applicable to the preparation of other materials with strict requirements.

Due to the characteristics of lithium-ion battery materials that are easy to be oxidized and easily adsorbed and modified by water vapor, it is determined that they cannot be exposed to the atmospheric environment during the preparation of lithium-ion battery materials and the observation of microscopic morphology. Lithium-ion battery materials were prepared in a glove box filled with a protective atmosphere of positive nitrogen gas and transferred to SEM for observation of the samples. The self-driven sample vacuum transfer system is placed in the glove box. The self-driven sample vacuum transfer system includes a vacuum box and a vacuum pump set, and the prepared sample is fixed on the sample holder. At this time, the box body is in the open state, as shown in Figures 5 to 8, and also referring to Figures 15 and 16, the sample holder with the sample fixed thereon can be inserted into the fixing groove of the self-driven ejection sample stage. At this time, the spring sleeved on the guide shaft is in an open state, as shown in FIG. 7 . Connect the air nozzle of the vacuum sealing valve and the vacuum pump group through the gas pipeline, and press the self-driven ejection sample stage into the box body. At this time, the spring sleeved on the guide shaft is in a compressed state, as shown in Figure 3. Start the vacuum pump group to vacuumize the box body, and close the vacuum sealing valve switch after reaching a certain degree of vacuum to keep the box body in a vacuum-sealed state. Take out the gas line from the air nozzle of the vacuum sealing valve, take out the vacuum box from the glove box, transfer it to the SEM sample chamber, and fix the vacuum box. During the mobile transfer, the sample is always fixed on the sample holder and vacuum sealed in the box. Close the SEM sample chamber and start the SEM vacuum system. When the SEM sample chamber reaches a certain degree of vacuum, the pressure difference between the vacuum box body 1 and the sample chamber is rapidly reduced, that is, the pressure of the SEM sample chamber decreases rapidly and keeps approaching the vacuum box body 1. Under the pressure of the compression spring, the self-driven pop-up sample stage is ejected by the elastic force of the compression spring, as shown in Figure 5 to Figure 8, and the sample can be observed and detected in the SEM in the next step. It can be seen from the above description that during the preparation, transfer and observation process, the sample is always in a protective atmosphere or a vacuum environment to maximize the isolation of the impact of air or water vapor on the sample; moreover, only the vacuum box is transferred, which has the advantage of small size . The whole process is cleverly controlled by vacuum pressure and elastic force, and no electric drive is required.

The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity, all possible combinations of the technical features in the above-described embodiments are not described. However, as long as there is no contradiction between the combinations of these technical features, All should be regarded as the scope described in this specification.

The above-mentioned embodiments only represent several embodiments of the present application, and the descriptions thereof are specific and detailed, but should not be construed as a limitation on the scope of the invention patent. It should be pointed out that for those skilled in the art, without departing from the concept of the present application, several modifications and improvements can be made, which all belong to the protection scope of the present application. Therefore, the scope of protection of the patent of the present application shall be subject to the appended claims.

Claims

A sample vacuum transfer system comprising:

vacuum pump unit; and

Vacuum box, including:

box body;

A self-driven ejection sample stage, the self-driven ejection sample stage is provided with a cover plate, a bracket member and an elastic member connected in sequence, one end of the elastic member is fixed inside the box body, and the other end is movably abutted against the bracket member;

Vacuum sealed valve body;

a vacuum seal valve air nozzle for connecting the vacuum pump set; and

a sample holder, detachably arranged on the bracket;

Wherein, when the elastic member is in a compressed state, the cover plate is in contact with the box body, the cover plate and the box body together form a closed cavity, and the bracket member is located in the cavity; When the elastic member is in a free state, the sample holder is located outside the box; the vacuum sealing valve body is respectively connected to the chamber and the air nozzle of the vacuum sealing valve.
The system of claim 1 , wherein the cover plate has a convex shape such that there is a space inside the cover plate that becomes part of the chamber.
The system of claim 1, wherein the box has a prismatic or cylindrical shape.
The system of claim 1, wherein the vacuum sealing valve body is disposed inside the casing and the vacuum sealing valve air nozzle is exposed outside the casing.
The system of claim 1, wherein the chamber is located inside the box body, the elastic member is in a compressed state, and the cover plate is in contact with the box body to close the chamber.
The system according to claim 1, wherein the vacuum sealing valve body is provided with a vacuum sealing valve switch, and the vacuum sealing valve switch is used to make the vacuum sealing valve in a closed state The body and the chamber are in a closed state or an open state.
The system according to claim 1, wherein the sample holder comprises a connected tray and a fixed end, the tray is used to carry the sample, the bracket member is provided with a fixed groove corresponding to the fixed end, the The fixing end is detachably fixed in the fixing groove, so that the tray is detachably arranged on the bracket member.
The system according to claim 1, wherein a sealing gasket is further provided on the box body or the cover plate, the cover plate is in contact with the box body through the sealing gasket when the elastic member is in a compressed state contact to close the chamber.
The system according to claim 1, wherein a resisting member is provided inside the box body.
The system according to claim 9, wherein the self-driven ejection sample stage is further provided with a guide shaft and a mounting portion, the mounting portion is fixed inside the box body, and one end of the guide shaft is fixed on the abutting member and the other end is fixed on the mounting part.
The system according to claim 10, wherein the bracket member is provided with an upper bracket, an inner bracket and a lower bracket connected in sequence, the guide shaft is arranged through the inner bracket, and one end of the elastic member is fixed to the abutment. On the holding piece, the other end is movably abutted against the inner bracket; the elastic piece is a hollow piece and the elastic piece is sleeved outside the guide shaft, and the elastic piece is in a telescopic state, so that the support piece can move along the inner frame. The guide shaft moves.
The system of claim 11, wherein the sample holder is detachably disposed on the upper support.
The system according to claim 11, wherein an upper guide rail and a lower guide rail are further provided inside the box body, the upper bracket is slidably arranged on the upper guide rail, and the lower bracket is slidably arranged on the lower guide rail.
The system according to claim 11, wherein the bracket member is further provided with an outer bracket, the upper bracket and the lower bracket are respectively connected with the outer bracket, and the outer bracket is connected with the cover plate.
The system according to claim 11, wherein the upper bracket is further provided with a positioning portion for fixing the sample holder under a certain force.
The system according to claim 11, wherein the bracket member is further provided with a middle bracket located between the outer bracket and the inner bracket, and the upper bracket and the lower bracket are respectively connected with the middle bracket , the guide shaft is also arranged through the middle bracket.
The system of claim 1, wherein the resilient member is a spring or a resilient block.
The system of claim 1, further comprising a pipe body through which the vacuum pump set is connected to the vacuum sealing valve air nozzle.
A sample vacuum transfer method comprising:

Provide the sample vacuum transfer system of claim 1;

Put the sample into the sample holder;

Put the sample holder on the support piece of the self-driven ejection stage;

pushing the support piece of the self-driven ejection stage into the cavity of the cassette and bringing the cover plate of the self-driven ejection stage into contact with the cassette to close the cavity;

The vacuum sealing valve body and the connected chamber are evacuated through the vacuum sealing valve air nozzle;

Close the vacuum seal valve valve; and

Transfer the vacuum box as a whole to the target platform.
The method according to claim 19, wherein after transferring the vacuum box as a whole to the target platform, further comprising vacuuming on the target platform until the elastic member of the self-driven ejection sample stage ejects the bracket member and the sample holder is located outside the box.