A multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment and its operation method

Abstract

The present invention discloses a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device and an operating method thereof, wherein the reaction chamber comprises a sealing cover and a base that are buckled together, wherein a first conductive fixing clamp and a second conductive fixing clamp are provided in parallel on the inner bottom plate of the base, wherein a sample fixing clamp is clamped and fixed between the first conductive fixing clamp and the second conductive fixing clamp, wherein electrodes are respectively mounted on both ends of a clamping plate on one side of the sample fixing clamp, and the electrodes at both ends are respectively in contact with and cooperate with the corresponding side clamps of the first conductive fixing clamp and the second conductive fixing clamp, wherein the sample is arranged between the clamping plates that are opposite to each other and the two ends of the sample are respectively in contact with and cooperate with the electrodes, and a cooling system is respectively provided on both sides of the sample fixing clamp. The present invention also discloses an operating method for a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device. The present invention can achieve a higher precursor loading amount and a faster cooling speed, and can also meet the requirements of preparing a sample vacuum environment and a variety of reaction atmospheres.

Description

Technical Field

[0001] The present invention belongs to the technical field of electrically triggered Joule heating devices, and in particular relates to a multifunctional and convenient reaction chamber for electrically triggered Joule heating devices and an operating method thereof. Background Art

[0002] Currently, electrically triggered Joule heating devices are widely used due to their rapid heating capabilities. For example, Professor Hu Liangbing of the University of Maryland successfully prepared a variety of nano-high-entropy alloys using this method (Science, 2018, 359(6383):1489). The preparation process is as follows: In an argon-filled glove box, a carbon fiber sheet impregnated with a metal precursor is connected to two copper electrodes coated with silver paste. A Keithley DC power supply then applies a pulsed current to the copper electrodes. The Joule heating effect of the current generates a transient high temperature on the carbon paper, reaching a maximum temperature of 2000K and lasting for approximately 55 milliseconds. This transient high temperature provides reaction conditions for the reduction of the metal precursor supported on the carbon fiber, resulting in the uniform dispersion of the resulting alloy on the carbon fiber surface. Electrically triggered Joule heating devices can also be used to prepare RGO, CNF, biomass carbon materials, and carbon cloth, providing a new method for the rapid and efficient synthesis of advanced functional nanomaterials and showing great potential for the preparation of advanced nanomaterials.

[0003] At present, there are still some problems and shortcomings in electrically triggered Joule heating equipment: 1. The rapid heating process will cause the metal precursors on the load and carbon fiber to quickly vaporize and splash, thereby reducing the metal loading; 2. Relying on natural cooling after power failure, it is difficult to achieve the preparation of amorphous alloys with high cooling rate requirements; 3. Some organic precursors will produce a large amount of gas during the rapid heating process, causing the pressure inside the reaction chamber to rise rapidly, posing an explosion risk. Summary of the Invention

[0004] In order to address the shortcomings and deficiencies of the above-mentioned electrically triggered Joule heating device, the present invention provides a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device and an operating method thereof. The multifunctional and convenient reaction chamber can not only increase the loading amount of substances required for the sample, but also enable the sample to be immediately cooled after rapid heating. In addition, the reaction chamber can also continuously introduce the required protective gas or maintain a vacuum state according to the requirements of different samples for the preparation environment.

[0005] In order to solve the above technical problems, the present invention adopts the following technical solutions: a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device, characterized in that it includes a sealing cover and a base that are buckled together, wherein a first conductive fixing clamp and a second conductive fixing clamp are provided on the inner bottom plate of the base in parallel, and a sample fixing clamp is clamped and fixed between the first conductive fixing clamp and the second conductive fixing clamp, and electrodes are respectively installed at both ends of a clamping plate on one side of the sample fixing clamp, and the electrodes at both ends are respectively in contact with the corresponding side clamps of the first conductive fixing clamp and the second conductive fixing clamp, the sample is set between the clamping plates arranged opposite to each other on the sample fixing clamp, and the two ends of the sample are respectively in contact with the electrodes, and a cooling system is provided on both sides of the sample fixing clamp, and the cooling system is composed of a push-pull electromagnet fixed on the inner side wall of the base and a push-pull electromagnet arranged to extend and retract. The cooling block is composed of a cooling block at one end, a liquid inlet hose and a liquid outlet hose connected to the liquid inlet and liquid outlet of the cooling block, and a liquid inlet pipe and a liquid outlet pipe that are sealed and pass through the bottom plate of the base and are respectively connected to the liquid inlet hose and the liquid outlet hose. The cooling block can be fitted with the clamps on both sides of the sample fixing clamp under the action of the push-pull electromagnet to cool the sample. The push-pull electromagnets on both sides are respectively connected to the controller through the wires that are sealed and pass through the bottom plate of the base. The clips in the first conductive fixing clamp and the second conductive fixing clamp that contact and cooperate with the electrodes are respectively connected to the controller through the wires that are sealed and pass through the bottom plate of the base. A vacuum tube, an air inlet pipe and an air outlet pipe that are sealed and pass through the bottom plate are provided on the bottom plate of the base. The vacuum tube is connected to the vacuum pump through an air valve and a vacuum pipeline, the air inlet pipe is connected to the air source through the air valve and the air inlet pipeline, and the air outlet pipe is connected to the exhaust pipeline through the air valve.

[0006] It is further defined that the first conductive fixing clamp and the second conductive fixing clamp are both composed of clips vertically fixed to the inner bottom plate of the base and arranged opposite to each other. The first conductive fixing clamp and the second conductive fixing clamp are both trumpet-shaped structures with a larger opening at the top and a smaller opening at the bottom, which are used to facilitate the clamping and unloading of the sample fixing clamp.

[0007] It is further defined that the gas source is one or more of a nitrogen source, an argon source, a hydrogen source, an oxygen source or an air source.

[0008] It is further defined that the cooling block is composed of a heat dissipation block and a heat dissipation pipe arranged inside the heat dissipation block, wherein the liquid inlet end of the heat dissipation pipe is connected to the liquid inlet hose through the liquid inlet, the liquid inlet pipe is connected to the liquid outlet of the circulating water tank through the liquid inlet pipeline and the water pump, the liquid outlet end of the heat dissipation pipe is connected to the liquid outlet hose through the liquid outlet, and the liquid outlet pipe is connected to the liquid inlet of the circulating water tank through the liquid outlet pipeline.

[0009] It is further defined that the structure of the heat dissipation pipe is spiral, S-shaped, right-angle bend or wavy, and the heat exchange medium flowing in the heat dissipation pipe is water.

[0010] It is further defined that the electrode is a copper electrode or a silver electrode.

[0011] The method for operating the multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment of the present invention is characterized by the following specific steps:

[0012] Step S1: Before starting work, all air valves are in a closed state, and the water pump, vacuum pump, push-pull electromagnet of the cooling system, and the clips connecting the electrodes in the first conductive fixing clamp and the second conductive fixing clamp are all controlled by a controller, and the controller switches of the relevant components are all in a closed state;

[0013] Step S2: placing the sample in the middle of the sample clamp, with both ends of the sample in contact with the electrodes on the sample clamp. Then, clamping the sample clamp containing the sample in the gap between the first conductive clamp and the second conductive clamp, with the sample clamp in contact with the first conductive clamp and the second conductive clamp, and with the electrodes on the sample clamp pressed tightly against the clips on the corresponding sides of the first conductive clamp and the second conductive clamp.

[0014] Step S3: After the sample inside the base is fixed, the sealing cover is fastened to the base. Then, according to the needs of sample preparation, the controller is adjusted to different preparation modes, wherein mode 1 is a preparation mode under vacuum state, i.e., the air valve on the vacuum line is opened and the vacuum pump is used to evacuate the reaction chamber; mode 2 is a preparation mode under different gas source atmospheres, i.e., the air valves on the air inlet line and the exhaust line are opened and the air inlet line is connected to the required gas source to switch the atmosphere in the reaction chamber;

[0015] Step S4: After the adjustment mode is reached, the controller is turned on, and the water pump is started synchronously. Cooling water flows in from the liquid inlet pipe, passes through the heat dissipation pipe in the cooling block, and then flows out from the liquid outlet pipe. The air in the liquid inlet pipe and the liquid outlet pipe is discharged in advance to ensure that the cooling water in the cooling block can continue to flow during operation.

[0016] Step S5: After the thermal shock is completed, the controller automatically turns on the cooling system, and the time jumps to the preset cooling time. Under the action of the push-pull electromagnet, the cooling block is attached to the two side clamps of the sample fixing clamp, and the sample is quickly cooled by heat conduction;

[0017] Step S6: After the cooling is completed, the controller will prompt and automatically start the water pump, and the push-pull electromagnet will reset. At this time, the controller switch will be turned off, the air valve will be closed at the same time, the sealing cover will be opened, the sample fixing clamp and the sample will be taken out, and the remaining cold water in the cooling block will be drained;

[0018] Step S7: Work completed, check again whether each controller switch and gas valve are completely closed.

[0019] Compared with the existing technology, the present invention has the following advantages and beneficial effects: compared with the traditional single-function heat-triggered Joule heating reaction chamber, the present invention can achieve a higher precursor loading capacity and a faster cooling speed, and can also meet the requirements of preparing sample vacuum environment and various reaction atmospheres. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 Schematic diagram of the overall structure of the reaction chamber;

[0021] Figure 2 Schematic diagram of the structure of the sealing cover in the reaction chamber;

[0022] Figure 3 is a top view of the base in the reaction chamber;

[0023] Figure 4 Schematic diagram of the internal structure of the base in the reaction chamber;

[0024] Figure 5 Schematic diagram of the bottom structure of the base in the reaction chamber;

[0025] Figure 6 is a top view of the sample fixing clamp in the reaction chamber;

[0026] Figure 7 is a side view of the sample fixing clamp in the reaction chamber;

[0027] Figure 8 Schematic diagram of the cooling block in the reaction chamber

[0028] Figure 9 Schematic diagram of the internal structure of the cooling block in the reaction chamber.

[0029] In the figure: 1-sealing cover, 2-base, 3-push-pull electromagnet, 4-liquid inlet hose, 5-liquid outlet hose, 6-air inlet pipe, 7-first conductive fixing clamp, 8-cooling block, 9-second conductive fixing clamp, 10-sample fixing clamp, 11-sample, 12-electrode, 13-liquid inlet pipe, 14-liquid outlet pipe, 15-wire, 16-vacuum tube, 17-air outlet pipe, 18-air valve. DETAILED DESCRIPTION

[0030] The specific technical content of the present invention is described in detail with reference to the accompanying drawings.

[0031] like Figure 1-9As shown, a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device comprises a sealing cover 1 and a base 2 which are buckled together, wherein a first conductive fixing clamp 7 and a second conductive fixing clamp 9 are provided on the inner bottom plate of the base 2 in parallel, and a sample fixing clamp 10 is clamped and fixed between the first conductive fixing clamp 7 and the second conductive fixing clamp 9, and electrodes 12 are respectively mounted on both ends of a clamping plate on one side of the sample fixing clamp 10, and the electrodes 12 at both ends are respectively in contact with the corresponding side clamps of the first conductive fixing clamp 7 and the second conductive fixing clamp 9, a sample 11 is provided between the oppositely arranged clamping plates of the sample fixing clamp 10, and both ends of the sample 11 are respectively in contact with the electrodes, and a cooling system is provided on both sides of the sample fixing clamp 10, and the cooling system consists of a push-pull electromagnet 3 fixed on the inner wall of the base 2, a cooling block 8 provided at the telescopic end of the push-pull electromagnet 3, and a liquid inlet and outlet connected to the cooling block 8. The sample 11 is cooled by the pressure relief valve 21 and the sample 11 is cooled by the pressure relief valve 22. The sample 11 is cooled by the pressure relief valve 21. The sample 11 is cooled by the pressure relief valve 22.

[0032] The first conductive fixing clamp 7 and the second conductive fixing clamp 9 of the present invention are both composed of clips vertically fixed to the inner bottom plate of the base 2 and arranged oppositely. The first conductive fixing clamp 7 and the second conductive fixing clamp 9 are both trumpet-shaped with a larger opening at the top and a smaller opening at the bottom, which are used to facilitate the clamping and unloading of the sample fixing clamp 10. The gas source is one or more of a nitrogen source, an argon source, a hydrogen source, an oxygen source or an air source. The cooling block 8 is composed of a heat dissipation block and a heat dissipation pipe arranged inside the heat dissipation block, wherein the liquid inlet end of the heat dissipation pipe is connected to the liquid inlet hose 4 through the liquid inlet, the liquid inlet pipe is connected to the liquid outlet of the circulating water tank through the liquid inlet pipeline and the water pump, the liquid outlet end of the heat dissipation pipe is connected to the liquid outlet hose 5 through the liquid outlet, and the liquid outlet pipe is connected to the liquid inlet of the circulating water tank through the liquid outlet pipeline. The structure of the heat dissipation pipe is spiral, S-shaped, right-angle bend or wavy, and the heat exchange medium circulating in the heat dissipation pipe is water. The electrode 12 is a copper electrode or a silver electrode. Example

[0033] A method for operating a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device, comprising the following steps:

[0034] (1) All air valves are manually controlled. The water pump, vacuum pump, cooling system, and the first and second conductive fixing clamps are all controlled by a controller, which has two different modes. Before starting work, all air valves and controller switches are in the closed state.

[0035] (2) Place the sheet sample in the middle of the sample holder, and make sure that the 5mm long parts at both ends of the sheet sample fit the copper electrodes on the sample holder (e.g. Figure 6 As shown), the assembled sample fixing clamp is then placed into the gap between the first conductive fixing clamp and the second conductive fixing clamp, so that the sample fixing clamp fits tightly against the first conductive fixing clamp and the second conductive fixing clamp, and the sample fixing clamp should press the copper electrode against the clips on the corresponding sides of the first conductive fixing clamp and the second conductive fixing clamp.

[0036] (3) After the sample inside the base is fixed, the sealing cover is tightly fastened to the base. Then the controller is adjusted to mode 2, and the argon gas inlet pipe valve and the argon gas exhaust pipe valve are opened. When the valve is opened, argon gas begins to be introduced into the reaction chamber. Argon gas is discharged into the reaction chamber from the inlet pipe and discharged from the reaction chamber into the water from the exhaust pipe. When obvious bubbles are seen in the water, the timing begins. The ventilation continues for about 1 minute to exhaust all the air in the reaction chamber.

[0037] (4) When the reaction chamber is filled with argon, turn on the controller switch to pass current, and perform electrically triggered Joule heating on the sheet sample within the preset time. When the controller is turned on, the water pump will also start synchronously. The cooling water flows in from the liquid inlet pipe, flows through the S-shaped heat dissipation pipe in the cooling block, and flows out from the liquid outlet pipe, exhausting the air in the pipe in advance to ensure that the cooling water in the cooling block can continue to flow during the working process.

[0038] (5) After the thermal shock is completed, the controller automatically turns on the cooling system, and the time jumps to the preset cooling time. Under the action of the push-pull electromagnet, the cooling block quickly fits against the sample clamp, and the sheet sample is quickly cooled by heat conduction;

[0039] (6) After the cooling is completed, the controller will prompt, the water pump will be turned off, and the push-pull electromagnet will return to its original position. At this time, turn off the controller switch, close the air valve, open the sealing cover, take out the sample fixing clamp and the sheet sample, and drain the remaining cold water in the cooling block;

[0040] (7) After the work is completed, check again whether all switches and gas valves are completely closed. Example

[0041] A method for operating a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device, comprising the following steps:

[0042] (1) All air valves are manually controlled. The water pump, vacuum pump, cooling system, and the first and second conductive fixing clamps are all controlled by a controller, which has two different modes. Before starting work, all air valves and controller switches are in the closed state.

[0043] (2) Place the sheet sample in the middle of the sample holder, and make sure that the 5mm long parts at both ends of the sheet sample fit the copper electrodes on the sample holder (e.g. Figure 6 As shown), the assembled sample fixing clamp is then placed into the gap between the first conductive fixing clamp and the second conductive fixing clamp, so that the sample fixing clamp is tightly fitted with the first conductive fixing clamp and the second conductive fixing clamp, and the sample fixing clamp is such that the copper electrode is pressed tightly with the clips on the corresponding sides of the first conductive fixing clamp and the second conductive fixing clamp;

[0044] (3) After the sample inside the base is fixed, the sealing cover is tightly fastened to the base, the controller is adjusted to mode 1, the air valve on the vacuum line is opened, and then the controller switch is turned on to start the vacuum pump. The air in the reaction chamber is extracted through the vacuum tube. When the controller is turned on, the water pump is also started synchronously. The cooling water flows into the liquid inlet pipe, flows through the S-shaped heat dissipation pipe in the cooling block, and flows out from the liquid outlet pipe. The air in the pipe is discharged in advance to ensure that the cooling water in the cooling block can flow continuously during operation.

[0045] (4) When the controller issues a prompt indicating that the reaction chamber is in a vacuum state, the vacuum pump automatically shuts down, and the controller displays the thermal shock time. The sample is electrically triggered to undergo Joule heating within the preset time, and the air valve on the vacuum line is closed while the thermal shock is occurring.

[0046] (5) After the thermal shock is completed, the controller automatically turns on the cooling system, and the time jumps to the preset cooling time. Under the action of the push-pull electromagnet, the cooling block quickly fits against the sample clamp, and the sheet sample is quickly cooled by heat conduction;

[0047] (6) After the cooling is completed, the controller will prompt, the water pump will be turned off, and the push-pull electromagnet will return to its original position. At this time, the controller switch will be turned off. Since the reaction chamber is in a vacuum state at this time, the sealing cover cannot be opened;

[0048] (7) Open the valves on the argon inlet pipe and the argon exhaust pipe. When the valves are opened, start to introduce argon into the reaction chamber. The argon is discharged from the inlet pipe into the reaction chamber and from the exhaust pipe out of the reaction chamber into the water. When obvious bubbles are seen in the water, open the sealing cover, remove the sample holder and the sheet sample, and drain the remaining cold water in the cooling block.

[0049] (8) After the work is completed, check again whether all switches and gas valves are completely closed.

[0050] The above embodiments describe the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for illustrating the principles of the present invention. Without departing from the scope of the principles of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of protection of the present invention.

Claims

1. A multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment, characterized in that The utility model comprises a sealing cover and a base which are buckled together, wherein a first conductive fixing clamp and a second conductive fixing clamp are provided in parallel on the inner bottom plate of the base, a sample fixing clamp is clamped and fixed between the first conductive fixing clamp and the second conductive fixing clamp, electrodes are respectively mounted on both ends of a clamping plate on one side of the sample fixing clamp, and the electrodes at both ends are respectively in contact with the corresponding side clamping pieces of the first conductive fixing clamp and the second conductive fixing clamp, the sample is arranged between the clamping plates which are arranged opposite to each other and the two ends of the sample are respectively in contact with the electrodes, a cooling system is respectively provided on both sides of the sample fixing clamp, and the cooling system consists of a push-pull electromagnet fixed on the inner wall of the base, a cooling block provided at the telescopic end of the push-pull electromagnet, and a liquid inlet hose connected to the liquid inlet and liquid outlet of the cooling block The sample fixing clamp is composed of a liquid outlet hose and a liquid inlet pipe and a liquid outlet pipe which are sealed and pass through the bottom plate of the base and are respectively connected to the liquid inlet hose and the liquid outlet hose, wherein the cooling block can be fitted with the clamps on both sides of the sample fixing clamp under the action of the push-pull electromagnet to achieve cooling of the sample, and the push-pull electromagnets on both sides are respectively connected to the controller through the wires which are sealed and pass through the bottom plate of the base, and the clips in the first conductive fixing clamp and the second conductive fixing clamp which are in contact with the electrodes are respectively connected to the controller through the wires which are sealed and pass through the bottom plate of the base, and a vacuum tube, an air inlet pipe and an air outlet pipe which are sealed and pass through the bottom plate are provided on the bottom plate of the base, wherein the vacuum tube is connected to the vacuum pump through an air valve and a vacuum pipeline, the air inlet pipe is connected to the air source through the air valve and the air inlet pipeline, and the air outlet pipe is connected to the exhaust pipeline through the air valve.

2. The multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment according to claim 1, characterized in that: The first conductive fixing clamp and the second conductive fixing clamp are both composed of clips vertically fixed to the inner bottom plate of the base and arranged opposite to each other. The first conductive fixing clamp and the second conductive fixing clamp are both trumpet-shaped structures with a larger opening at the top and a smaller opening at the bottom, which are used to facilitate the clamping and unloading of the sample fixing clamp.

3. The multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment according to claim 1, characterized in that: The gas source is one or more of a nitrogen gas source, an argon gas source, a hydrogen gas source, an oxygen gas source or an air gas source.

4. The multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment according to claim 1, characterized in that: The cooling block is composed of a heat dissipation block and a heat dissipation pipe arranged inside the heat dissipation block, wherein the liquid inlet end of the heat dissipation pipe is connected to the liquid inlet hose through the liquid inlet, the liquid inlet pipe is connected to the liquid outlet of the circulating water tank through the liquid inlet pipeline and the water pump, the liquid outlet end of the heat dissipation pipe is connected to the liquid outlet hose through the liquid outlet, and the liquid outlet pipe is connected to the liquid inlet of the circulating water tank through the liquid outlet pipeline.

5. The multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment according to claim 4, characterized in that: The structure of the heat dissipation pipe is spiral, S-shaped, right-angle bend or wave-shaped, and the heat exchange medium flowing in the heat dissipation pipe is water.

6. The multifunctional and convenient reaction chamber for electrically triggered Joule heating equipment according to claim 1, characterized in that: The electrodes are copper electrodes or silver electrodes.

7. A method for operating a multifunctional and convenient reaction chamber for an electrically triggered Joule heating device according to claim 4, characterized in that The specific steps are: Step S1: Before starting work, all air valves are in a closed state, and the water pump, vacuum pump, push-pull electromagnet of the cooling system, and the clips connecting the electrodes in the first conductive fixing clamp and the second conductive fixing clamp are all controlled by a controller, and the controller switches of the relevant components are all in a closed state; Step S2: placing the sample in the middle of the sample clamp, with both ends of the sample in contact with the electrodes on the sample clamp. Then, clamping the sample clamp containing the sample in the gap between the first conductive clamp and the second conductive clamp, with the sample clamp in contact with the first conductive clamp and the second conductive clamp, and with the electrodes on the sample clamp pressed tightly against the clips on the corresponding sides of the first conductive clamp and the second conductive clamp. Step S3: After the sample inside the base is fixed, the sealing cover is fastened to the base. Then, according to the needs of sample preparation, the controller is adjusted to different preparation modes, wherein mode 1 is a preparation mode under vacuum state, i.e., the air valve on the vacuum line is opened and the vacuum pump is used to evacuate the reaction chamber; mode 2 is a preparation mode under different gas source atmospheres, i.e., the air valves on the air inlet line and the exhaust line are opened and the air inlet line is connected to the required gas source to switch the atmosphere in the reaction chamber; Step S4: After the adjustment mode is reached, the controller is turned on, and the water pump is started synchronously. Cooling water flows in from the liquid inlet pipe, passes through the heat dissipation pipe in the cooling block, and then flows out from the liquid outlet pipe. The air in the liquid inlet pipe and the liquid outlet pipe is discharged in advance to ensure that the cooling water in the cooling block can continue to flow during operation. Step S5: After the thermal shock is completed, the controller automatically turns on the cooling system, and the time jumps to the preset cooling time. Under the action of the push-pull electromagnet, the cooling block is attached to the two side clamps of the sample fixing clamp, and the sample is quickly cooled by heat conduction; Step S6: After the cooling is completed, the controller will prompt and automatically start the water pump, and the push-pull electromagnet will reset. At this time, the controller switch will be turned off, the air valve will be closed at the same time, the sealing cover will be opened, the sample fixing clamp and the sample will be taken out, and the remaining cold water in the cooling block will be drained; Step S7: Work completed, check again whether each controller switch and gas valve are completely closed.

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