A device for in-situ degassing of a physical adsorption instrument

Abstract

The utility model provides a kind of device for in-situ degassing of physical adsorption instrument, including box, heating mechanism, lifting mechanism, dewar flask, sample bottle and degassing analysis mechanism The box is equipped with baffle, and the inner part of box is separated into operating area, installation area and analysis area by baffle, and analysis area is above operating area and installation area, and the heating mechanism and lifting mechanism are installed to installation area, and the heating furnace of heating mechanism and the lifting tray of lifting mechanism are set in operating area, and the dewar flask is placed in lifting tray;The degassing analysis mechanism is installed to analysis area, and sample bottle is installed to the fixed end of degassing analysis mechanism, and the heating furnace of heating mechanism can realize the heating of sample bottle.The utility model solves the problems of complex operation, low efficiency, sample contamination, uneven heating, high equipment failure rate and other problems in the traditional physical adsorption instrument degassing device.

Description

Technical Field

[0001] This utility model belongs to the field of physical adsorption instruments, and in particular relates to a device for in-situ degassing of physical adsorption instruments. Background Technology

[0002] For over a century since Langmuir discovered that the physical adsorption of nitrogen molecules on a solid surface at liquid nitrogen temperatures could be used to measure the specific surface area of ​​solid materials, physical adsorption technology has been widely used for the analysis of specific surface area and pore structure of solid materials. Currently, common physical adsorption testing procedures require measuring the adsorption amount of the sample at a predetermined target pressure. By using the adsorption data at a series of pressure points, the specific surface area and pore distribution of the sample can be calculated. Before testing, actual samples adsorb moisture and other impurities from the air. The presence of these impurities affects both sample quality and the adsorption capacity measurement. Therefore, samples must be degassed before physical adsorption analysis. Typically, the degassing device is separate from the analytical device to prevent impurities removed during degassing from entering the analytical section's piping and contaminating the piping and sensors, thus affecting the accuracy of the analytical data. For these independent degassing stations, the sample is first degassed by heating and vacuuming. After degassing, the sample tube is removed and weighed under protective backfill gas before being installed in the analytical station for analysis. Under normal circumstances, the weighing and installation process can be completed quickly. Because of the protective gas, air is unlikely to enter the sample tube and cause secondary contamination; therefore, this is the standard operating procedure for the instrument.

[0003] With the development of materials science, some new materials require an absolutely anhydrous and oxygen-free environment during synthesis, and after synthesis, they need to be stored in a solvent to ensure that the sample is isolated from water, oxygen, and other atmospheres. For such samples, trace amounts of water, oxygen, and other atmospheres diffuse into the sample tube during the weighing process after ex-situ degassing, which may damage the sample structure and render the test data invalid.

[0004] Therefore, an in-situ degassing device is needed so that the sample can be degassed without having to be removed for weighing or transfer, and can then be used in the analysis process, thus protecting the sample from damage.

[0005] Currently, there are two main approaches to in-situ degassing: The first type of instrument is mostly an integrated structure of analysis and degassing with independent internal pipelines. In this case, the undegassed sample can be installed in the analysis station, and the heating pack configured in the degassing station can be fixed on the outside of the sample tube for heating. At the same time, the sample can be evacuated through manual control mode, which can also complete the in-situ degassing operation. This approach does not require altering the original instrument structure and is suitable for occasional use, but it is cumbersome to operate. The heating pack cable has a limited length, and special care must be taken when wrapping the sample. The degassing process requires manual control of the solenoid valve, which places high demands on the operator.

[0006] The second type features a Dewar flask elevator in its instrument analysis station equipped with a rotatable dual-tray configuration. One tray holds the Dewar flasks for the analysis process, while the other tray holds the heating furnace for sample pretreatment. This enables in-situ degassing of the samples. This design alters the original instrument structure, occupies a large space, and the heating furnace, with its heating and temperature acquisition wiring, needs to rotate back and forth on a rotating tray, posing a certain risk of malfunction with long-term use. The closed-loop heating furnace used has slow heat dissipation; after degassing, a lengthy cooling process is required before the furnace can be removed, the Dewar raised, and subsequent analysis can proceed, severely impacting the instrument's efficiency. Utility Model Content

[0007] In view of this, the present invention aims to propose an in-situ degassing device for a physical adsorption instrument, which solves the problems of complex operation, low efficiency, easy sample contamination, uneven heating, and high equipment failure rate in traditional physical adsorption instrument degassing devices.

[0008] To achieve the above objectives, the technical solution of this utility model is implemented as follows: A device for in-situ degassing in a physical adsorption apparatus includes a housing, a heating mechanism, a lifting mechanism, a Dewar flask, sample vials, and a degassing analysis unit. The chamber is equipped with a partition that divides the interior of the chamber into an operation area, an installation area, and an analysis area. The analysis area is located above the operation area and the installation area. The heating mechanism and the lifting mechanism are installed in the installation area. The heating furnace of the heating mechanism and the lifting tray of the lifting mechanism are located in the operation area. The Dewar flask is placed on the lifting tray. The degassing analysis unit is installed in the analysis area, and the sample vials are installed at the fixed end of the degassing analysis unit. The heating furnace of the heating mechanism is capable of heating the sample vials.

[0009] Furthermore, the heating mechanism includes a first drive motor, a counter-rotating screw, a first connecting arm, a second connecting arm, a first heating furnace, and a second heating furnace; The housing has mounting plates on both sides, with a slide rail and opposing screws between the two mounting plates. The No. 1 drive motor is also mounted on the mounting plate. The output end of the No. 1 drive motor has a drive wheel, and the end of the opposing screw has a driven wheel. The drive wheel and the driven wheel are connected by a synchronous belt. The first end of the No. 1 connecting arm is connected to the opposing screw, and the second end is equipped with the No. 1 heating furnace; the first end of the No. 2 connecting arm is connected to the opposing screw, and the second end is equipped with the No. 2 heating furnace.

[0010] Furthermore, the first connecting arm and the second connecting arm have the same structure. The first end of the first connecting arm and the second connecting arm are provided with a sliding block. The sliding block is threadedly connected to the opposing screw and slides with the slide rail, so as to realize the opposing or backward movement of the first connecting arm and the second connecting arm, thereby realizing the closing or opening of the first heating furnace and the second heating furnace.

[0011] Furthermore, both the No. 1 heating furnace and the No. 2 heating furnace are semi-cylindrical in shape, and when closed, they form a cylindrical shape. The distance between the No. 1 and No. 2 heating furnaces when they are fully open is greater than the outer diameter of the Dewar flask.

[0012] Furthermore, the lifting mechanism includes a lifting motor, a lifting seat, a lifting screw, a lifting guide rod, a lifting block, and a lifting tray; The lifting seat is installed onto the housing, and the parallel lifting screw and lifting guide rod are installed onto the lifting seat. A lifting motor is located on the top of the lifting seat. The output end of the lifting screw is connected to the lifting motor. The lifting block and the lifting screw are threaded together, and the lifting block is slidably connected to the lifting guide rod. The lifting tray is installed on the lifting block, and the Dewar bottle is placed on the lifting tray to drive the lifting of the Dewar bottle.

[0013] Furthermore, the Dewar flask has an opening at the top, allowing the sample tube to enter the flask when it rises.

[0014] Compared with existing technologies, the in-situ degassing device for physical adsorption described in this utility model has the following advantages: (1) The device for in-situ degassing of a physical adsorption instrument described in this utility model completes the two key steps of "degassing" and "analysis" in the same device, reducing the intermediate steps such as sample transfer, weighing, and reinstallation caused by the separation of the degassing station and the analysis station in the traditional method. It automates the operation, improves experimental efficiency, reduces human error, and ensures the integrity of the sample.

[0015] (2) The device for in-situ degassing of a physical adsorption instrument described in this utility model does not interfere with the volatilization of liquid nitrogen in the Dewar flask during the heating process, ensuring the compatibility of the degassing process with the low temperature environment and expanding the application range of the device.

[0016] (3) The device for in-situ degassing of a physical adsorption instrument described in this utility model has a heating furnace with a two-piece opening and closing design. It has a simple structure and no complex rotating or frequently moving parts. Compared with the rotating tray or long cable heating pack in the existing solution, it has a lower failure rate, is more convenient to maintain, and has a longer service life. Attached Figure Description

[0017] The accompanying drawings, which form part of this utility model, are used to provide a further understanding of the utility model. The illustrative embodiments of the utility model and their descriptions are used to explain the utility model and do not constitute an undue limitation of the utility model. In the drawings: Figure 1 This is a schematic diagram of an in-situ degassing device for a physical adsorption apparatus according to an embodiment of the present invention; Figure 2 This is a schematic diagram of the hidden housing of the in-situ degassing device for a physical adsorption instrument according to an embodiment of the present invention; Figure 3 This is a schematic diagram of the heating mechanism described in an embodiment of the present utility model; Figure 4 This is a schematic diagram of the lifting mechanism described in an embodiment of the present utility model.

[0018] Explanation of reference numerals in the attached figures: 1. Chamber; 2. Heating mechanism; 21. Drive motor No. 1; 22. Opposing screw; 23. Connecting arm No. 1; 24. Connecting arm No. 2; 25. Heating furnace No. 1; 26. Heating furnace No. 2; 3. Lifting mechanism; 31. Lifting motor; 32. Lifting seat; 33. Lifting screw; 34. Lifting guide rod; 35. Lifting block; 36. Lifting tray; 4. Dewar flask; 5. Sample bottle; 6. Degassing analysis mechanism. Detailed Implementation

[0019] It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other.

[0020] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, are only for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the invention. Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0021] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art will understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0022] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0023] A device for in-situ degassing using a physical adsorption apparatus, such as Figures 1-4 As shown, it includes a housing 1, a heating mechanism 2, a lifting mechanism 3, a Dewar flask 4, a sample bottle 5, and a degassing analysis mechanism 6. The heating mechanism 2, the lifting mechanism 3, and the degassing analysis mechanism 6 are all connected to a controller. The degassing analysis mechanism 6 is a prior art technology. The housing 1 is equipped with a partition, which divides the interior of the housing 1 into an operation area, an installation area and an analysis area. The analysis area is above the operation area and the installation area. The heating mechanism 2 and the lifting mechanism 3 are installed in the installation area. The heating furnace of the heating mechanism 2 and the lifting tray 36 of the lifting mechanism 3 are located in the operation area. The Dewar flask 4 is placed on the lifting tray 36. The degassing analysis unit 6 is installed in the analysis area, and the sample bottle 5 is installed at the fixed end of the degassing analysis unit 6. The heating furnace of the heating mechanism 2 can heat the sample bottle 5.

[0024] The enclosure 1 is divided into three functional areas: operation, installation, and analysis by partitions, which helps to improve operational safety and experimental efficiency and avoid mutual interference. The degassed sample does not need to be removed and can be tested directly in the analysis area, avoiding contamination and errors caused by sample transfer and improving the accuracy and reliability of test data.

[0025] Preferably, the heating mechanism 2 includes a first drive motor 21, a counter-rotating screw 22, a first connecting arm 23, a second connecting arm 24, a first heating furnace 25, and a second heating furnace 26; The housing 1 has mounting plates on both sides, and a slide rail and a counter-rotating screw 22 are provided between the two mounting plates. The first drive motor 21 is also mounted on the mounting plate. The output end of the first drive motor 21 is provided with a drive wheel, and the end of the counter-rotating screw 22 is provided with a driven wheel. The drive wheel and the driven wheel are connected by a synchronous belt. The first end of the first connecting arm 23 is connected to the opposing screw 22, and the second end is equipped with the first heating furnace 25; the first end of the second connecting arm 24 is connected to the opposing screw 22, and the second end is equipped with the second heating furnace 26.

[0026] The heating furnace is automatically opened and closed by a motor drive, eliminating the need for manual adjustment, thus completing the automated operation, reducing reliance on operators, and improving experimental efficiency and consistency.

[0027] Preferably, the first connecting arm 23 and the second connecting arm 24 have the same structure. The first end of the first connecting arm 23 and the second connecting arm 24 are provided with a sliding block. The sliding block is threadedly connected to the opposing screw 22 and slides in cooperation with the slide rail, so as to realize the opposing or backward movement of the first connecting arm 23 and the second connecting arm 24, thereby realizing the closing or opening of the first heating furnace 25 and the second heating furnace 26.

[0028] Preferably, both the No. 1 heating furnace 25 and the No. 2 heating furnace 26 are semi-cylindrical in shape, and when closed, they form a cylindrical shape. After the semi-cylindrical heating furnace is closed, it can tightly wrap the sample tube, achieve 360° uniform heating, improve degassing efficiency and effect, and is particularly suitable for materials with high requirements for temperature field uniformity. When the No. 1 heating furnace 25 and the No. 2 heating furnace 26 are fully opened, the distance between them is greater than the outer diameter of the Dewar flask 4. Sufficient space is reserved when fully open to ensure that the Dewar flask 4 can be smoothly put in or removed. The opening and closing process of the heating furnace will not interfere with the Dewar flask 4, ensuring smooth operation.

[0029] Preferably, the lifting mechanism 3 includes a lifting motor 31, a lifting seat 32, a lifting screw 33, a lifting guide rod 34, a lifting block 35, and a lifting tray 36; The lifting seat 32 is installed on the housing 1, and the parallel lifting screw 33 and lifting guide rod 34 are installed on the lifting seat 32. The top of the lifting seat 32 is equipped with a lifting motor 31. The output end of the lifting screw 33 is connected to the lifting motor 31. The lifting block 35 and the lifting screw 33 are threadedly connected, and the lifting block 35 is slidably connected to the lifting guide rod 34. The lifting tray 36 is installed on the lifting block 35, and the Dewar bottle 4 is placed on the lifting tray 36 to realize the driving of lifting the Dewar bottle 4.

[0030] Preferably, the Dewar flask 4 has a mouth at the top, and when the Dewar flask 4 is raised, the sample tube can enter the Dewar flask 4.

[0031] Working principle: The sample to be tested is loaded into the sample bottle 5, which is installed at the fixed end of the degassing analysis mechanism 6. The Dewar bottle 4 is placed on the lifting tray 36 in the operating area of ​​the box 1, and is in the initial low position. During degassing, the No. 1 drive motor 21 drives the No. 1 heating furnace 25 and the No. 2 heating furnace 26 to close, heating the sample bottle 5. The heating process does not affect the evaporation of liquid nitrogen in the Dewar flask 4. The degassing operation is completed under the operation of the degassing analysis mechanism 6. After degassing, there is no need to wait for the furnace to cool down. The No. 1 heating furnace 25 and the No. 2 heating furnace 26 can be directly separated. Waiting for ten minutes will ensure that the sample temperature drops to room temperature, and subsequent analysis operations can begin. During analysis, the driving lifting motor 31 is activated to lift the Dewar flask 4, allowing the sample vial 5 to enter the Dewar flask 4, and then the analysis of the sample is completed by the degassing analysis mechanism 6.

[0032] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A device for in-situ degassing using a physical adsorption apparatus, characterized in that: Includes the chamber, heating mechanism, lifting mechanism, Dewar flask, sample vials, and degassing analysis mechanism. The chamber is equipped with a partition that divides the interior of the chamber into an operation area, an installation area, and an analysis area. The analysis area is located above the operation area and the installation area. The heating mechanism and the lifting mechanism are installed in the installation area. The heating furnace of the heating mechanism and the lifting tray of the lifting mechanism are located in the operation area. The Dewar flask is placed on the lifting tray. The degassing analysis unit is installed in the analysis area, and the sample vials are installed at the fixed end of the degassing analysis unit. The heating furnace of the heating mechanism is capable of heating the sample vials.

2. The device for in-situ degassing of a physical adsorption apparatus according to claim 1, characterized in that: The heating mechanism includes a first drive motor, a counter-rotating screw, a first connecting arm, a second connecting arm, a first heating furnace, and a second heating furnace; The housing has mounting plates on both sides, with a slide rail and opposing screws between the two mounting plates. The No. 1 drive motor is also mounted on the mounting plate. The output end of the No. 1 drive motor has a drive wheel, and the end of the opposing screw has a driven wheel. The drive wheel and the driven wheel are connected by a synchronous belt. The first end of the No. 1 connecting arm is connected to the opposing screw, and the second end is equipped with the No. 1 heating furnace; the first end of the No. 2 connecting arm is connected to the opposing screw, and the second end is equipped with the No. 2 heating furnace.

3. The device for in-situ degassing of a physical adsorption apparatus according to claim 2, characterized in that: The first connecting arm and the second connecting arm have the same structure. The first end of the first connecting arm and the second connecting arm are provided with a sliding block. The sliding block is threadedly connected to the opposing screw and slides with the slide rail, so as to realize the opposite or backward movement of the first connecting arm and the second connecting arm, thereby realizing the closing or opening of the first heating furnace and the second heating furnace.

4. The device for in-situ degassing of a physical adsorption apparatus according to claim 3, characterized in that: Both the No. 1 heating furnace and the No. 2 heating furnace are semi-cylindrical in shape, and when closed, they form a cylindrical shape. The distance between the No. 1 and No. 2 heating furnaces when they are fully open is greater than the outer diameter of the Dewar flask.

5. The device for in-situ degassing of a physical adsorption apparatus according to claim 1, characterized in that: The lifting mechanism includes a lifting motor, a lifting seat, a lifting screw, a lifting guide rod, a lifting block, and a lifting tray; The lifting seat is installed onto the housing, and the parallel lifting screw and lifting guide rod are installed onto the lifting seat. A lifting motor is located on the top of the lifting seat. The output end of the lifting screw is connected to the lifting motor. The lifting block and the lifting screw are threaded together, and the lifting block is slidably connected to the lifting guide rod. The lifting tray is installed on the lifting block, and the Dewar bottle is placed on the lifting tray to drive the lifting of the Dewar bottle.

6. The apparatus for in-situ degassing of a physical adsorption instrument according to claim 5, characterized in that: The Dewar flask has an opening at the top, and when the Dewar flask is raised, the sample tube can enter the Dewar flask.

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