CN219625401U - Inert atmosphere sample injection device for vacuum sample injection cavity - Google Patents

Abstract

The utility model relates to an inert atmosphere sample injection device for a vacuum sample injection cavity, which comprises a glove box and a vacuum sample injection cavity, wherein the surface of the glove box is provided with an air inlet, an air outlet, a glove connecting port, a sample injection door. The back of glove box is equipped with the biography appearance mouth, be equipped with flange joint spare in the biography appearance mouth, the glove box passes through flange joint spare and vacuum sampling cavity UNICOM, flange joint spare is including the axial pass the two-sided edge of a knife flange of biography appearance mouth. According to the utility model, the flange connecting piece with the rapid sample injection door is arranged on one side of the inert atmosphere sample injection device and is connected with the glove box through the flange connecting piece, so that when advanced surface characterization is carried out, an air-sensitive sample can be prevented from contacting with water, carbon dioxide, oxygen and the like in the air in the transmission process from preparation to entering the test cavity, the authenticity and reliability of a sample surface test result are ensured, and the influence on experimental data caused by sample deterioration is prevented.

Description

Inert atmosphere sample injection device for vacuum sample injection cavity

Technical Field

The utility model belongs to the technical field of X-ray spectrum and electron spectrum testing, and particularly relates to an inert atmosphere sample injection device for a vacuum sample injection cavity.

Background

The advanced surface characterization techniques that are currently more common are: x-ray photoelectron spectroscopy (XPS), X-ray angular resolved photoelectron spectroscopy (ARPES), scanning Electron Microscopy (SEM), transmission Electron Microscopy (TEM), synchronous radiation soft X-ray absorption spectroscopy (sXAS) and the like, and the method is mainly used for carrying out test analysis on the morphology and the electronic structure of the surface of a material in the depth range of 2-100nm, and is very sensitive to the surface state of the material.

However, many energy and catalytic materials, particularly secondary battery materials, contain active metals such as lithium and sodium and high-valence transition metal elements, and when exposed directly to air, react rapidly with oxygen, carbon dioxide, water vapor and the like in the air, resulting in deterioration. Even a short exposure time, the reaction products on the surface can seriously affect the test results of the surface detection means.

At present, most of conventional experimental equipment is used for testing air-sensitive materials by packaging the materials in a glove box of a laboratory, disassembling a sample after the materials arrive at a testing site, and rapidly transferring the sample into a vacuum sampling cavity of the equipment. This method also results in a sample exposed to air for 30-60 seconds at best, and the material is still subject to unavoidable deterioration due to brief exposure to air, which does not guarantee the accuracy of the characterization. Therefore, there is an urgent need to design an inert atmosphere sample injection device to realize the nondestructive transfer of samples from a laboratory glove box to a test vacuum cavity.

Disclosure of Invention

The utility model aims to solve the technical problem of providing an inert atmosphere sampling device for a vacuum sampling cavity, so that a sample can be directly fed into the inert atmosphere sampling device and subjected to surface detection under the condition of not contacting with air.

The technical scheme adopted for solving the technical problems is as follows: an inert atmosphere sample injection device for a vacuum sample injection cavity is provided, and comprises a glove box and a vacuum sample injection cavity, wherein the surface of the glove box is provided with an air inlet, an air outlet, a glove connecting port and a sample injection door. The back of glove box is equipped with the biography appearance mouth, pass appearance mouth and hollow flange joint spare seal link to each other, the glove box passes through flange joint spare and vacuum sampling cavity UNICOM, flange joint spare is including the axial pass the two-sided edge of a knife flange of biography appearance mouth, two-sided edge of a knife flange is located one side periphery welding in the glove box has annular metal sheet and passes through edge of a knife flange sealing connection with quick sampling door, annular metal sheet with the inboard sealing connection of glove box, one side that two-sided edge of a knife flange is located the glove box passes through edge of a knife flange sealing connection with vacuum sampling cavity.

Further, the glove box is a rectangular box, the glove connecting port is arranged on the front face of the glove box, the sample inlet is arranged on the side face of the glove box, a sample table is arranged in the center of the glove box, and the flange connecting piece is arranged on the back face of the glove box.

Further, the glove box is filled with an inert atmosphere through the air inlet, and the inert atmosphere is a nitrogen atmosphere or an argon atmosphere.

Further, an oxygen detector and a humidity detector are arranged in the glove box.

Further, the sample inlet door is a sealing plate with a handle, and the sealing plate is detachably and hermetically assembled on the glove box through screws and sealing rubber rings.

Further, one side that annular metal sheet with the glove box meets is equipped with the annular groove, be equipped with O type sealing washer in the annular groove, be equipped with a plurality of sealed screw thread blind holes on the annular metal sheet, one side periphery cover that two-sided edge of a knife flange is located the glove box is outside has the holding ring, be equipped with on the holding ring with sealed screw thread through-hole that sealed screw thread blind hole matches, pass appearance mouth periphery be equipped with sealed screw thread blind hole and sealed screw thread through-hole match's through-hole, the annular metal sheet pass through the bolt with O type sealing washer with glove box inboard sealing connection.

Advantageous effects

According to the inert atmosphere sample injection device for the vacuum sample injection cavity, the special flange connector with the rapid sample injection door is arranged on one side of the vacuum sample injection cavity, and the vacuum sample injection cavity is connected with the glove box, so that when advanced surface characterization is carried out, air-sensitive samples can be prevented from contacting with water, carbon dioxide, oxygen and the like in the air in the transmission process from preparation to entering the test cavity, the authenticity and the reliability of the test result of the sample surface are ensured, and the influence on experimental data caused by sample deterioration is prevented.

Drawings

FIG. 1 is a schematic diagram of an inert atmosphere injection device for a vacuum injection chamber.

Fig. 2 is an exploded view of the flange connector of fig. 1.

Fig. 3 is a schematic diagram of the glove box in fig. 1.

Fig. 4 is a perspective view of the double-sided knife edge flange of fig. 2.

Wherein, 1-glove box; a 2-flange connection; 3-a vacuum sample injection cavity; 4-a rapid sample injection door; 5-a double-sided knife edge flange; 6-a ring-shaped metal plate; 7-O-shaped sealing rings; 8-fastening rings; 9. 10-copper washer; 11-a sample injection cavity flange; 12-sample transferring port; 13-air inlet; 14-exhaust port; 15-glove connection port; 16-sample injection gate.

Detailed Description

The utility model will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present utility model and are not intended to limit the scope of the present utility model. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present utility model, and such equivalents are intended to fall within the scope of the utility model as defined in the appended claims.

As shown in fig. 1, the utility model provides an inert atmosphere sample injection device for a vacuum sample injection cavity, which comprises a glove box 1, wherein the surface of the glove box 1 is provided with an air inlet 13, an air outlet 14, a glove connecting port 15 and a sample injection door 16, the back of the glove box 1 is provided with a sample transmission port 12, the sample transmission port 12 is in sealing connection with a hollow flange connecting piece 2, and the glove box 1 is communicated with the vacuum sample injection cavity 3 through the flange connecting piece 2. As shown in fig. 2 and 4, the flange connector 2 includes a double-sided knife edge flange 5 axially penetrating through the sample port 12, an annular metal plate 6 is welded on the periphery of one side of the double-sided knife edge flange 5 located in the glove box 1 and is in sealing connection with the rapid sample inlet 4 through the knife edge flange, the annular metal plate 6 is in sealing connection with the inner side of the glove box 1 through an O-shaped sealing ring 7, and one side of the double-sided knife edge flange 5 located outside the glove box 1 is in sealing connection with the vacuum sample inlet 3 through the knife edge flange.

As shown in fig. 3, the glove box 1 is a laboratory apparatus in which an inert gas is filled into a box body and the active material therein is circulated and filtered, and generally has two glove connection ports 15. In one embodiment, the front side of the glove box 1 is provided with an observation window, so that an operator can clearly observe the operation process in the box, and the air inlet 13 and the air outlet 14 are provided with connectors and valves, so that the air inlet and the air outlet can be connected with external equipment when air suction or air inflation is required.

In a specific embodiment, the rapid sampling door 4 is a standard CF63 shutter, the inside is sealed by an O-ring 7 made of elastic fluororubber, and the outside is clamped by an adjustable bolt during air suction, and the vacuum degree can reach 10 ^-8 mbar. See the patent: a sealing device with a pressure relief protection function (application number 201720665992.9) can be conveniently and rapidly connected with a flange.

In a specific embodiment, the knife edge flange sealing connection means that knife edges are arranged between flanges, the flanges are fastened by bolts, and copper gaskets 9 and 10 are inserted between two adjacent knife edges to realize sealing connection.

In a specific embodiment, the glove box 1 is a rectangular box, the glove connection port 15 is disposed on the front surface of the glove box 1, the sample inlet 16 is disposed on the side surface of the glove box 1, a sample stage is disposed in the center of the glove box 1, and the flange connector 2 is disposed on the back surface of the glove box 1.

In a specific embodiment, the glove box 1 is filled with an inert atmosphere through the air inlet 13, and the internal air is exhausted through the air outlet 14, wherein the inert atmosphere is a nitrogen atmosphere or an argon atmosphere.

In a specific embodiment, an oxygen detector and a humidity detector are arranged in the glove box 1, the inert atmosphere environment in the glove box 1 is detected at any time, the condition that the water and oxygen content in the glove box reaches the standard is ensured, then the sample is unsealed, and the sample is transported after the inert atmosphere meets the requirement.

In a specific embodiment, the sample inlet door 16 is a sealing plate with a handle, 8 matched threaded holes are formed in the sample inlet door 16 and the glove box 1, and the sealing plate is detachably and hermetically assembled on the glove box 1 through a screw and a sealing rubber ring when the sample inlet door 16 is closed.

In a specific embodiment, an annular groove is formed in one side, connected with the glove box 1, of the annular metal plate 6, an O-shaped sealing ring 7 is arranged in the annular groove, a plurality of sealing threaded blind holes are formed in the annular metal plate 6, a fastening ring 8 is sleeved on the periphery of one side, located outside the glove box 1, of the double-sided knife edge flange 5, a sealing threaded through hole matched with the sealing threaded blind holes is formed in the fastening ring 8, a through hole matched with the sealing threaded blind holes and the sealing threaded through hole is formed in the periphery of the sample conveying port 12, and the annular metal plate 6 is in sealing connection with the inner side of the glove box 1 through bolts and the O-shaped sealing ring 7. Since the blind sealing thread does not penetrate the annular metal plate 6, gas leakage at the threaded connection can be better prevented.

The utility model comprises the following steps when in use: firstly, placing an air-sensitive sample which is well sealed into a glove box 1 through a sample inlet door 16; then the exhaust port 14 is started to exhaust, and the air inlet 13 is started to input inert gas; after the water oxygen content in the glove box reaches a very low value, under the condition of maintaining the circulation of inert atmosphere, opening a sample package in the glove box 1 and sending the sample into the vacuum sample injection cavity 3 through the flange connector 2 by the rapid sample injection door 4; closing the rapid sample injection door 4 to raise the vacuum degree in the vacuum sample injection cavity 3 to be lower than 10 ^-4 Exhausting can be stopped after mbar; the sample can be transferred into the test cavity without contacting with airAdvanced surface characterization.

Claims (6)

1. The utility model provides an inert atmosphere sampling device for vacuum sampling chamber, is equipped with air inlet (13) including the surface, gas vent (14), glove connector (15), glove box (1) and vacuum sampling chamber (3) of sampling door (16), its characterized in that, the back of glove box (1) is equipped with and passes appearance mouth (12), it links to each other with hollow flange joint spare (2) seal to pass appearance mouth (12), glove box (1) is passed through flange joint spare (2) and vacuum sampling chamber (3) UNICOM, flange joint spare (2) include the axial pass two-sided knife edge flange (5) of appearance mouth (12), two-sided knife edge flange (5) are located one side periphery welding in glove box (1) has annular metal sheet (6) and passes through knife edge flange sealing connection with quick sampling door (4), annular metal sheet (6) with the inboard sealing connection of glove box (1), one side that two-sided knife edge flange (5) are located outside glove box (1) passes through knife edge flange sealing connection with vacuum sampling chamber (3).

2. The inert atmosphere sample injection device for a vacuum sample injection cavity according to claim 1, wherein the glove box (1) is a rectangular box, the glove connection port (15) is arranged on the front surface of the glove box (1), the sample injection door (16) is arranged on the side surface of the glove box (1), a sample table is arranged in the center of the glove box (1), and the flange connection piece (2) is arranged on the back surface of the glove box (1).

3. An inert atmosphere injection device for a vacuum injection chamber according to claim 2, characterized in that the glove box (1) is filled with an inert atmosphere through the gas inlet (13), the inert atmosphere being a nitrogen atmosphere or an argon atmosphere.

4. The inert atmosphere sampling device for the vacuum sampling cavity according to claim 2, wherein an oxygen detector and a humidity detector are arranged in the glove box (1).

5. An inert atmosphere injection device for a vacuum injection cavity according to claim 1, characterized in that the injection door (16) is a sealing plate with a handle, and the sealing plate is detachably and hermetically assembled on the glove box (1) through screws and sealing rubber rings.

6. The inert atmosphere sampling device for a vacuum sampling cavity according to claim 1, characterized in that an annular groove is formed in one side, connected with a glove box (1), of the annular metal plate (6), an O-shaped sealing ring (7) is arranged in the annular groove, a plurality of sealing threaded blind holes are formed in the annular metal plate (6), a fastening ring (8) is sleeved on the periphery of one side, located outside the glove box (1), of the double-sided knife edge flange (5), a sealing threaded through hole matched with the sealing threaded blind hole is formed in the fastening ring (8), a through hole matched with the sealing threaded blind hole and the sealing threaded through hole is formed in the periphery of a sample conveying port (12), and the annular metal plate (6) is in sealing connection with the inner side of the glove box (1) through bolts and the O-shaped sealing ring (7).