Large device for testing interconnection characterization of branch-linked matrix atmosphere box

Abstract

The invention discloses a large device for testing interconnection characterization of a branch-linked matrix atmosphere box. The large device comprises atmosphere box units, a branch-linked matrix interconnection system, a central control system, an inert gas circulation system, a safety monitoring system and a characterization testing module. Material transfer and atmosphere sharing among a plurality of atmosphere box units are realized through a branch-linked matrix interconnection system, and meanwhile, physical and chemical characterization test functions are integrated, so that the requirements of efficient synthesis preparation and real-time monitoring of a new energy battery material are met. The characterization test module has the main technical indexes of an integrated microscopic CT characterization test system, an atomic force microscope measurement system, a charge and discharge electrochemical performance test system, a super field depth microscope measurement system, an in-situ X-ray diffraction characterization test system, a contact angle measurement system and a Fourier transform infrared spectrum characterization test system. The laser microscopic Raman spectrum characterization testing system and the ultraviolet-visible spectrum analysis testing system are used for carrying out physical, chemical or optical characterization testing on materials.

Description

Technical Field

[0001] The present invention relates to an inert atmosphere box device, and particularly to a large device for interconnected characterization testing of a branched matrix atmosphere box, which is applicable to the transfer of highly reactive chemical materials, the characterization testing of materials, and the experimental or production fields of material synthesis and preparation that need to be carried out in an inert atmosphere environment. Background Art

[0002] With the rapid development of the new energy industry, the demand for the upgrade of new energy battery technology is becoming increasingly urgent. However, the main raw materials for the synthesis of new energy batteries (such as active metals like lithium and sodium) are highly sensitive to air and are prone to oxidation, hydrolysis and other reactions in the air, seriously affecting the performance and safety of materials. Therefore, the synthesis and preparation process of new energy batteries and their materials need to be carried out in an inert atmosphere environment. At present, most of the existing inert atmosphere box devices are glove boxes with independent units, which have the following problems: 1. It is impossible to achieve material transfer and atmosphere sharing between multiple atmosphere boxes, resulting in low experimental efficiency; 2. Lack of integrated physical and chemical characterization testing functions, making it difficult to monitor and analyze material properties in real time; 3. Low degree of automation and complex operation, making it difficult to meet the needs of large-scale production and scientific research experiments. Summary of the Invention

[0003] To solve the above problems, the present invention proposes a large device for interconnected characterization testing of a branched matrix atmosphere box, which realizes material transfer, atmosphere sharing and integrated physical and chemical characterization testing functions between multiple atmosphere box units through a branched matrix interconnection system and a central control system, and at the same time integrates physical and chemical characterization testing modules to achieve efficient synthesis and preparation of new energy battery materials. The specific component modules of the large device include:

[0004] Module 1 Atmosphere Box Unit

[0005] Module 2 Branched Matrix Interconnection System

[0006] Module 3 Central Control System

[0007] Module 4 Inert Gas Circulation System

[0008] Module 5 Safety Monitoring System

[0009] Module 6 Characterization Testing System

[0010] Preferably, in Module 1 Atmosphere Box Unit, each atmosphere box unit includes a sealed working cavity, an inert gas supply system and a gas purification system; the box body is made of SUS304 stainless steel, equipped with a detachable safety glass window and an aluminum alloy glove port.

[0011] Preferably, in the module 2 branched matrix interconnection system, material transfer between multiple atmosphere chamber units is achieved through sealable connecting pipes, material transfer cabins, and valve control devices.

[0012] Preferably, in the module 3 central control system, Siemens PLC and touch screen control are adopted to achieve automatic adjustment of the box pressure, gas composition, and temperature.

[0013] Preferably, in the module 4 inert gas circulation system, the circulation and monitoring of inert gas are achieved through gas circulation pumps and gas composition analyzers.

[0014] Preferably, in the module 5 safety monitoring system, oxygen sensors, humidity sensors, and pressure sensors are equipped to monitor the atmosphere state of the box in real time.

[0015] Preferably, in the module 6 characterization and testing module, a micro-CT characterization and testing system, an atomic force microscope measurement system, a charge-discharge electrochemical performance testing system, a super-depth-of-field microscope measurement system, an in-situ X-ray diffraction characterization and testing system, a contact angle measurement system, a Fourier transform infrared spectroscopy characterization and testing system, a laser micro-Raman spectroscopy characterization and testing system, and an ultraviolet-visible spectroscopy analysis and testing system are integrated for physical, chemical, or optical characterization and testing of materials. Specific implementation mode

[0016] It is designed to consist of 11 groups of special structure atmosphere boxes and 1 group of automatic transmission system channels. Among the 11 groups of atmosphere boxes, 3 groups are atmosphere boxes for optical detection environment systems, 4 groups are interconnected preparation atmosphere boxes, and 4 groups are environment characterization system atmosphere boxes.

[0017] Step 1: According to the scientific research experiments required for the samples to be processed, the experimenter can select any atmosphere box to put the samples in for experiments.

[0018] Step 2: After the experiment in Step 1 is completed, the experimenter can take out the samples through the large and small chambers of the atmosphere box to complete the experimental work. If it is necessary to continue with the next scientific research experiment, the experimenter can directly choose to put the samples into the carrier vehicle of the automatic transmission system channel and transfer them to any of the other 10 groups of atmosphere boxes through the track for the next scientific research experiment.

[0019] Step 3: After the experiment in Step 2 is completed, the experimenter can take out the samples through the large and small chambers of the atmosphere box to complete the experimental work. If it is necessary to continue with the next scientific research experiment, the experimenter can directly choose to put the samples into the carrier vehicle of the automatic transmission system channel and transfer them to any of the other 10 groups of atmosphere boxes through the track for the next scientific research experiment.

[0020] After the experiment in Step 4 and Step 3 is completed, the experimenter can take out the samples through the large and small chambers of the atmosphere chamber to finish the experimental work. If it is necessary to continue with the next scientific research experiment, the samples can be directly placed into the carrier vehicle of the automatic transmission system channel and transported through the track to any one of the other 10 atmosphere chambers for the next scientific research experiment.

[0021] …… until the experimental task is completed. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The attached drawings forming a part of the present invention are used to provide a further understanding of the present invention. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. Obviously, for those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative efforts.

[0023] Figure 1 It is the general design drawing of a large device for characterizing the interconnection of a dendritic matrix atmosphere chamber of the present invention;

[0024] Figure 2 It is the design drawing of the automatic transmission device of the dendritic matrix interconnection system of the present invention.

[0025] Figure 3 It is the design drawing of the atmosphere chamber unit of the present invention.

[0026] Specific Composition Structure

[0027] Structure 1: Automatic Transmission System Device

[0028] I. The system consists of a set of inert gas transmission system and a complete set of transmission mechanisms.

[0029] II. Box

[0030] 1. The box body has dimensions of 16000 mm (length) × 450 mm (width) × 500 mm (height), and is divided into six sections connected by flanges. The box body material is SUS304 stainless steel with a thickness of 3 mm.

[0031] 2. Removable safety glass window, with an inclined operation surface, and the tempered glass has a thickness of 8 mm.

[0032] 3. Aluminum alloy glove port, processed from solid bar stock.

[0033] 4. Butyl rubber gloves.

[0034] 5. Customized anti-collision device for the glove port.

[0035] 6. Lighting system is installed at the top of the window.

[0036] 7. Safety valve to protect the equipment and the materials inside the glove box.

[0037] 8. Steel structure support, equipped with universal casters.

[0038] 9. The box body has a certain anti-seismic function design.

[0039] III. Transmission System

[0040] 1. The transfer glove box has an automatic material transfer system, and item transfer between any two glove boxes and equipment can be achieved through button jogging operation.

[0041] 2. Connection between each glove box and the transfer glove box through a transition chamber can avoid mutual contamination of different atmospheres.

[0042] 3. The transfer trolley is driven by a servo motor and uses a rack and pinion drive, with stable operation, high positioning accuracy, and a transmission accuracy better than ±1 mm.

[0043] 4. The imported linear guide of the transmission system should avoid generating dust particles.

[0044] 5. The transfer trolley is small, compact, and flexible, with reliable performance of imported accessories. It can transfer items with a size of ≤Φ180mm * 300mm and a weight of ≤1 kg, and is controlled by a stepper motor rack and pinion and PLC, enabling material transfer between any two glove boxes.

[0045] 6. The transmission system is automatically controlled by PLC, with autonomous positioning and one-key calling, making the operation convenient.

[0046] 7. The transmission system should be convenient for maintenance and have expandability in the later stage.

[0047] 8. In the later stage, the material transfer distance can be extended only by extending the track.

[0048] 9. Flanges for future expansion are reserved at both ends for future expansion channels.

[0049] 10. The transmission system and the glove box system can be integrated into the customer's central control system.

[0050] 1) The glove box is controlled by PLC plus a touch screen, and the PLC is Siemens SMART 200.

[0051] 2) The main parameter information and alarm information of the transmission system and the glove box can be monitored.

[0052] 3) An Ethernet data interface (standard RJ45) is provided, supporting communication protocols such as Siemens standard GET / PUT and OPC.

[0053] 4) Remote control can be supported.

[0054] IV. Gas Purification System

[0055] 1. One gas purification column:

[0056] ①Select high-performance copper catalysts and molecular sieves that are most suitable for gas purification in the glove box for water and oxygen removal.

[0057] ②The adsorption amounts of oxygen and water are 120 liters and 4 kg respectively.

[0058] 2. After the gas purification column is adsorbed saturated, it is regenerated with hydrogen-containing nitrogen or argon to restore its adsorption capacity.

[0059] ①Use a hydrogen / nitrogen mixture as the regeneration gas. H2: 4.1%; N2: 95.9%.

[0060] 3. One circulation fan

[0061] ①Flow rate: 60 m3 / h.

[0062] ②Installed in a sealed stainless-steel container, the stainless-steel container is made by full welding, with good sealing performance.

[0063] 4. Renewable organic solvent adsorption column

[0064] ①Containing activated carbon particle adsorption material.

[0065] ○2 Can be regenerated after adsorption saturation.

[0066] 5. Electrically pneumatically controlled circulation main valve, KF40 standard interface.

[0067] 6. All gas circuits are controlled by solenoid valves, and the regeneration of the purification column is fully automatically controlled.

[0068] 7. Gas filters are installed at the inlet and outlet of the circulation system.

[0069] V. Control System

[0070] 1. The control system consists of a Siemens PLC and a 7" color touch screen.

[0071] 2. Realize the following control functions:

[0072] 1) Automatically control the box pressure

[0073] a) The working pressure range can be arbitrarily set between +10 and -10 mbar, and the PLC will automatically regulate the box pressure within the set range. The default value of the working pressure range is 0 to +5 mbar.

[0074] b) When the box pressure is greater than 12 mbar, the PLC automatically opens the safety valve to relieve pressure to protect the gloves, equipment and materials in the box.

[0075] c) Use the foot switch to finely adjust the box pressure.

[0076] 2) The transition cabin can be evacuated and filled with gas multiple times with a single key, saving time.

[0077] Users can set the evacuation and filling times, evacuation time per operation, and filling pressure, and then start the automatic evacuation and filling program to complete the evacuation and filling automatically within the set time.

[0078] 3) The cycle purification can be automatically controlled by the water and oxygen indicators inside the box, greatly extending the lifespan of the fan, reducing the temperature inside the glove box, and saving energy.

[0079] 4) The leakage rate can be monitored manually or automatically.

[0080] a) Set manual detection: Just press the start detection button, and the PLC will automatically detect the airtightness of the box and report the leakage rate of the box.

[0081] b) Set automatic monitoring. The PLC will automatically detect the leakage of the box and report the leakage rate at the set time every day according to the user's settings. If the set value is exceeded, the system will pop up a window warning the user that the leakage rate exceeds the standard. This can timely detect situations such as damaged gloves and sealing strips.

[0082] 5) Automatic gas cleaning function inside the box

[0083] Users set the cleaning time and touch the start button on the touch screen, and the system will start cleaning the box and automatically stop at the set time.

[0084] 6) The system automatically records and displays historical data, and can also export the data within a specific time, such as box pressure, water content, and oxygen content, using a USB flash drive.

[0085] 7) Display operation errors and prompts

[0086] 8) Automatic alarm for the atmosphere inside the box

[0087] 9) All operations have preset conditions and action interlocks to avoid damage to the equipment or disruption of the atmosphere inside the box due to unsafe operations.

[0088] The leakage rate of the glove box can be automatically monitored: Set automatic monitoring. The PLC will automatically detect the leakage of the box and report the leakage rate at the set time every day according to the user's settings. If the set value is exceeded, the system will pop up a window warning the user that the leakage rate exceeds the standard. This can timely detect situations such as damaged gloves and sealing strips.

[0089] V. Internet of Things control system:

[0090] 1) Remote real-time monitoring function, displaying all contents on the touch control screen of the glove box

[0091] a) Monitorable data: Box pressure, oxygen content, water content.

[0092] b) Monitorable status: regeneration working status, working status of each solenoid valve, alarm status.

[0093] 2) Remote real-time control function. Through the "real-time configuration" function, all controllable components on the glove box touch control screen can be remotely manipulated.

[0094] a) Operable buttons: lighting, fan, vacuum pump, box cleaning.

[0095] b) Operable loop parameter setting: manual / automatic mode switching, manual mode switch, upper limit of oxygen content, lower limit of oxygen content, upper limit of water content, lower limit of water content.

[0096] c) Operable system parameter setting: cleaning time, pumping and filling times, upper limit of box pressure, lower limit of box pressure, upper limit of oxygen alarm, upper limit of water alarm.

[0097] Structure 2: Optical detection environment system

[0098] I. System composition structure

[0099] It includes three inert gas systems with dimensions of 2.4 * 1.2 * 0.9 meters, namely Fourier transform infrared spectroscopy characterization test system, laser micro Raman spectroscopy characterization test system, and ultraviolet-visible spectroscopy analysis test system.

[0100] II. Box body

[0101] 1. The box body has dimensions of 2400mm (length) X 1200mm (width) X 900mm (height), and the box body material is SUS304 stainless steel with a thickness of 3mm.

[0102] 2. Removable safety glass window, inclined operating surface, and the tempered glass has a thickness of 8mm.

[0103] 3. Eight aluminum alloy glove ports, machined from solid bars.

[0104] 4. Eight butyl rubber gloves.

[0105] 5. The box body side plate is reserved with eight KF40 standard interfaces.

[0106] 6. Customized anti-collision device for glove ports.

[0107] 7. Lighting system is installed at the top of the window.

[0108] 8. Safety valve to protect the equipment and materials inside the glove box.

[0109] 9. Steel structure bracket, installed with universal casters.

[0110] 10. The box body has a certain seismic function design.

[0111] 11. Double-layer partition rack

[0112] 12. A large airlock

[0113] 1) Material: SUS304 stainless steel, thickness 3mm

[0114] 2) Dimensions: Φ370X600mm

[0115] 3) Location: On the right side of the box

[0116] 4) Connection method: Flange connection

[0117] 5) Conveying method: Through a moving tray, the tray is easily detachable, facilitating the transfer of large-sized materials

[0118] 6) Operating method

[0119] a) Manual operation: Touch the valve through the touch screen

[0120] b) Automatic operation: With automatic air extraction and inflation functions, the user only needs to touch the start button on the touch screen, and the PLC automatically completes multiple pumping and filling procedures, standardizes the operation, saves time, and improves work efficiency. The user can set the number of pumping and filling times, the air extraction time each time, and the inflation pressure

[0121] 13. A small airlock

[0122] 1) Material: SUS304 stainless steel, thickness 4mm

[0123] Dimensions: Φ150X300mm

[0124] 3) Location: On the right side of the box

[0125] Connection method: Welding, no leakage, no seal aging problem

[0126] Conveying method: Through a moving tray

[0127] 6) Operating method: Manual operation through a three-way ball valve

[0128] 14. A docking small airlock

[0129] 1) Material: SUS304 stainless steel, thickness 4mm

[0130] 2) Dimensions: Φ200X400mm

[0131] 3) Location: On the left side of the box

[0132] III. Three sets of gas purification systems

[0133] The functional parameters are the same as those of the gas purification system in the automatic transmission system

[0134] IV. Three sets of control systems

[0135] The functional parameters are the same as those of the control system in the automatic transmission system

[0136] V. Internet of Things control system:

[0137] The functional parameters are the same as those of the Internet of Things control system in the automatic transmission system

[0138] Structure 3: Interconnected preparation system

[0139] I. System composition structure

[0140] The system includes four inert gas systems with dimensions of 1.2 * 1.2 * 0.9 meters, namely a disassembly system, an assembly system, an in-situ X-ray diffraction characterization test system, and a contact angle measurement system

[0141] II. Chamber

[0142] 1. The chamber size is 1200mm (length) X 1200mm (width) X 900mm (height), and the chamber material is SUS304 stainless steel with a thickness of 3mm

[0143] steel, with a thickness of 3mm

[0144] 2. Removable safety glass window, with an inclined operating surface, and the tempered glass thickness is 8mm

[0145] 3. Four aluminum alloy glove ports, machined from solid bars

[0146] 4. Four butyl rubber gloves

[0147] 5. Four KF40 standard interfaces are reserved on the side plate of the chamber

[0148] 6. Customized anti-collision device for the glove port

[0149] 7. Lighting system is installed at the top of the window

[0150] 8. Safety valve to protect the equipment and materials inside the glove box

[0151] 9. Steel structure support, equipped with universal casters

[0152] 10. The chamber has a certain seismic function design

[0153] 11. Double-layer partition shelf

[0154] 12. One large transfer chamber

[0155] 1) Material: SUS304 stainless steel, thickness 3mm

[0156] 2) Size: Φ370X600mm

[0157] 3) Location: on the right side of the box

[0158] 4) Connection method: flange connection

[0159] 5) Conveying method: through a movable tray, the tray is easily detachable, facilitating the transfer of large-sized materials

[0160] 6) Operation method

[0161] a) Manual operation: touch the valve through the touch screen

[0162] b) Automatic operation: with automatic air extraction and inflation functions, the user only needs to touch the start button on the touch screen, and the PLC automatically completes multiple air extraction and inflation procedures, standardizing the operation, saving time, and improving work efficiency. The user can set the number of air extraction and inflation times, the air extraction time each time, and the inflation pressure.

[0163] 13. A small transition chamber

[0164] 1) Material: SUS304 stainless steel, thickness 4mm.

[0165] 1) Dimensions: Φ150X300mm

[0166] 3) Location: on the right side of the box

[0167] 4) Connection method: welded, leak-free, no sealing aging problem

[0168] 5) Conveying method: through a movable tray

[0169] 6) Operation method: manual operation through a three-way ball valve

[0170] 14. A docking small transition chamber

[0171] 1) Material: SUS304 stainless steel, thickness 4mm.

[0172] 2) Dimensions: Φ200X400mm

[0173] 3) Location: on the left side of the box

[0174] III. Four sets of gas purification systems

[0175] The functional parameters are the same as those of the gas purification system in the automatic transmission system

[0176] IV. Four sets of control systems

[0177] The functional parameters are the same as those of the control system in the automatic transmission system

[0178] V. Internet of Things control system:

[0179] The functional parameters are the same as those of the Internet of Things control in the automatic transmission system

[0180] Structure 4: Environmental Characterization System

[0181] I. System Composition Structure

[0182] The system includes four inert atmosphere systems with dimensions of 1.5 * 1.2 * 0.9 meters, namely a micro-CT characterization test system, an atomic force microscope measurement system, a charge-discharge electrochemical performance test system, and a super-depth-of-field microscope measurement system.

[0183] II. Box

[0184] 1. The box has dimensions of 1500 mm (length) X 1200 mm (width) X 900 mm (height), and the box material is SUS304 stainless

[0185] steel, with a thickness of 3 mm.

[0186] 2. A detachable safety glass window and an inclined operating surface, with the tempered glass having a thickness of 8 mm.

[0187] 3. Six aluminum alloy glove ports, machined from solid bars.

[0188] 4. Six butyl rubber gloves.

[0189] 5. Eight KF40 standard interfaces are reserved on the side plate of the box.

[0190] 6. A customized anti-collision device for the glove port.

[0191] 7. A lighting system is installed at the top of the window.

[0192] 8. A safety valve to protect the equipment and the materials inside the glove box.

[0193] 9. A steel structure bracket equipped with universal casters.

[0194] 10. The box has a certain seismic function design.

[0195] 11. A double-layer shelf.

[0196] 12. A large transfer chamber

[0197] 1) Material: SUS304 stainless steel, with a thickness of 3 mm.

[0198] 2) Dimensions: Φ370X600 mm

[0199] 3) Location: On the right side of the box

[0200] 4) Connection method: Flange connection

[0201] 5) Transfer method: Through a movable tray, and the tray is easily detachable to facilitate the transfer of large-sized materials

[0202] 6) Operating mode

[0203] a) Manual operation: Touch the valve through the touch screen

[0204] b) Automatic operation: It has the functions of automatic air extraction and inflation. The user only needs to touch the start button on the touch screen, and the PLC automatically completes multiple air extraction and inflation procedures, with standardized operation, time saving and improved work efficiency. The user can set the number of air extraction and inflation times, the air extraction time each time and the inflation pressure.

[0205] 13. A small transition chamber

[0206] 1) Material: SUS304 stainless steel, thickness 4mm.

[0207] 2) Dimensions: Φ150X300mm

[0208] 3) Location: On the right side of the box

[0209] 4) Connection method: Welded, no leakage, no sealing aging problem. 5) Transfer method: Through a moving tray

[0210] 6) Operating mode: Manual operation through a three-way ball valve. 14. A docking small transition chamber

[0211] 1) Material: SUS304 stainless steel, thickness 4mm.

[0212] 2) Dimensions: Φ200X400mm

[0213] 3) Location: On the left side of the box

[0214] III. Four sets of gas purification systems

[0215] The function parameters are the same as those of the gas purification system in the automatic transfer system. IV. Four sets of control systems

[0216] The function parameters are the same as those of the control system in the automatic transfer system

[0217] V. Internet of Things control system:

[0218] The function parameters are the same as those of the Internet of Things control system in the automatic transfer system.

Claims

1. A large device for interconnected characterization testing of a branched matrix atmosphere chamber, characterized in that, It includes an atmosphere chamber unit, a branch-connected matrix interconnection system, a central control system, an inert gas circulation system, a safety monitoring system, and a characterization and testing module. Through the branch-connected matrix interconnection system and the central control system, material transfer, atmosphere sharing, and integrated characterization and testing functions are achieved among multiple atmosphere chamber units.

2. The device according to claim 1, characterized in that, The atmosphere chamber unit is made of SUS304 stainless steel and is equipped with a detachable safety glass window and an aluminum alloy glove port.

3. The device according to claim 1, characterized in that, The branch-connected matrix interconnection system realizes material transfer among multiple atmosphere chamber units through sealable connecting pipes and a material transfer cabin.

4. The device according to claim 1, characterized in that, The central control system is controlled by Siemens PLC and a touch screen to achieve automatic regulation of the box pressure, gas composition, and temperature.

5. The device according to claim 1, characterized in that, The inert gas circulation system is equipped with a gas circulation pump and a gas composition analyzer to achieve the circulation and monitoring of inert gas. High-performance copper catalysts and molecular sieve gas purification columns are used for water and oxygen removal.

6. The device according to claim 1, characterized in that The safety monitoring system is equipped with an oxygen sensor, a humidity sensor, and a pressure sensor to monitor the atmosphere state of the box in real time, achieve automatic leak detection and alarm functions, and ensure experimental safety.

7. The device according to claim 1, wherein The characterization and testing module integrates a micro-CT characterization and testing system, an atomic force microscope measurement system, a charge-discharge electrochemical performance testing system, a super-depth-of-field microscope measurement system, an in-situ X-ray diffraction characterization and testing system, a contact angle measurement system, a Fourier transform infrared spectroscopy characterization and testing system, a laser micro-Raman spectroscopy characterization and testing system, and an ultraviolet-visible spectroscopy analysis and testing system, which are used for physical, chemical, and other aspects of characterization and testing of materials, support real-time data recording and analysis, and improve experimental efficiency.

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