CN202471554U - Hydrogen diffusion and permeability measuring device - Google Patents

Abstract

The utility model discloses a hydrogen diffusion and permeation characteristic measuring device, which comprises a diffusion and permeation reactor with a first chamber and a second chamber, a gas supply system and a measurement system, and the hydrogen diffusion and permeation characteristic measuring device is also There is a heating system for heating the diffusion osmosis reactor. The utility model provides a heating system for the diffusion and penetration reactor, and the measurement device can measure and study the diffusion and penetration characteristics of hydrogen in high-temperature molten salt and solid materials.

Description

Measuring device for hydrogen diffusion and permeability characteristics

technical field

The utility model relates to a measuring device, in particular to a hydrogen diffusion and permeation characteristic measuring device.

Background technique

The molten salt reactor is one of the six types of reactors that are prioritized for the development of the fourth-generation nuclear energy system. Since the LiF molten salt reacts with neutrons in the molten salt reactor, a large amount of tritium (T) is produced, so the generated tritium (T) must be removed. Disposal to reduce impact on environment and test material. Tritium in the molten salt reactor mainly exists in the form of HT and TF. At high temperature, HT has strong permeability and is easy to seep out of the pipeline and cause pollution to the environment. TF is highly corrosive, and corrosion of pipeline materials will reduce the performance of pipeline materials. , affecting the safe operation of the reactor. In order to effectively remove different forms of tritium from molten salt, the diffusion and permeation behavior of different forms of tritium in molten salt and solid materials must be studied. Since both H (hydrogen) and T (tritium) are isotopes of hydrogen and have similar physical and chemical properties, stable nuclide hydrogen (H) can be used instead of radionuclide tritium (T) to study the diffusion of tritium in molten salts and solid materials Osmotic properties and chemical form transitions.

Among the previous methods of measuring hydrogen diffusion and permeation through test materials, the most important is the high-pressure gas-phase hydrogen permeation technology. Figure 1 shows a schematic diagram of a commonly used measurement device. The main device consists of a high-pressure chamber 13 and a low-pressure chamber 15. The sample 14 is placed between the high-pressure chamber 13 and the low-pressure chamber 15. Before measurement, the entire system is evacuated with a molecular pump, and then hydrogen is introduced from the gas cylinder 11 through the leak valve 12. In the high-pressure chamber, the gas enters the low-pressure chamber 15 from the sample to be tested 14 through the pressure difference, and the pressures of the two chambers are measured by the pressure gauges 16 and 17 respectively, so as to calculate the diffusion and permeation parameters of hydrogen through the test material. This device generally has the following disadvantages: first, there is no feeding port for filling the test material, so the test material cannot be replaced. Second, there is no heating device used in conjunction with the high-pressure chamber 13 and the low-pressure chamber 15, so it is impossible to measure the diffusion and penetration characteristics of hydrogen in high-temperature molten salts and solid materials, and it is also impossible to study the diffusion characteristics of hydrogen as temperature parameters change and permeability properties. Third, there is no device for processing TF, which affects the service life and safety of the test device. Fourth, the test system only uses the pressure gauges 16 and 17 to measure the pressure of the two chambers, and the measurement accuracy is limited due to the limitation of the measurement sensitivity of the instrument itself. Fifth, there is no real-time vacuuming device for the gas pipeline, so it is inconvenient to use.

Utility model content

The technical problem to be solved by the utility model is to provide a hydrogen diffusion and penetration characteristic measurement device in order to overcome the defect that the hydrogen diffusion and penetration characteristic measurement device in the prior art cannot measure and study the diffusion and penetration characteristics of hydrogen in high-temperature molten salt, The hydrogen diffusion and permeation characteristic measurement device can measure and study the diffusion and permeation characteristics of hydrogen in high-temperature molten salt.

The utility model solves the problems of the technologies described above through the following technical solutions:

A device for measuring hydrogen diffusion and permeation characteristics, which includes a diffusion and permeation reactor with a first chamber and a second chamber, a gas supply system and a measurement system, and is characterized in that the device for measuring hydrogen diffusion and permeation characteristics also has A heating system for heating the diffusion osmosis reactor.

Preferably, the heating system is a tubular resistance furnace with a heating tank, and the diffusion osmosis reactor is arranged in the heating tank.

Preferably, a nickel plate is provided at the interface between the first chamber and the second chamber.

Preferably, the measuring device further includes a feeding pipe and a molten salt adding part connected to one end of the feeding pipe, the other end of the feeding pipe communicates with the first chamber, and the pipe wall of the feeding pipe It is airtightly connected with the penetrating part of the first chamber. By providing a molten salt adding component communicated with the first chamber, the measuring device can conveniently update the test material.

Preferably, the device for measuring hydrogen diffusion and permeability characteristics further includes a vacuum suction component communicating with the first chamber and the second chamber. By setting the vacuum component, the measuring device can vacuumize the gas pipeline in real time, so it is convenient to use.

Preferably, the measurement system includes a detection component for detecting the temperature in the diffusion osmosis reactor. By setting the detecting component, the measuring device can measure the temperature parameter more accurately.

Preferably, the detection component is a thermocouple.

Preferably, the gas supply system includes an argon gas supply part and a hydrogen gas supply part, both of the argon gas supply part and the hydrogen gas supply part communicate with the first chamber and the second chamber. Since argon can be used as a carrier gas of hydrogen and can dilute hydrogen, the arrangement of the argon supply part facilitates the introduction of hydrogen and enables the measuring device to test the diffusion characteristics and permeation characteristics of hydrogen at different concentrations.

Preferably, both the argon gas supply part and the hydrogen gas supply part communicate with the first chamber and the second chamber through pipelines, and the vacuum suction part communicates with the first chamber and the second chamber through pipelines These pipelines are connected with pipeline valves. By setting these pipeline valves, it is convenient to control the gas in the pipeline, and the gas can be stopped to facilitate the replacement of local components.

Preferably, the hydrogen diffusion and permeability measurement device also includes a gas chromatograph and an HF gas absorption cell, the gas chromatograph is connected to the HF gas absorption cell through a six-way valve, and the six-way valve is also connected to the second The two chambers are connected. By setting the HF gas absorption pool, the service life and safety of the test device are increased. In addition, the use of the gas chromatograph greatly improves the test accuracy.

Preferably, the measurement system also includes four flowmeters and two pressure gauges, these flowmeters are respectively a flowmeter for measuring the argon flow rate supplied by the argon gas supply part, and a flowmeter for measuring the flow rate of the hydrogen gas supplied by the hydrogen gas supply part. A flow meter for the flow rate, a flow meter for measuring the gas output of the first chamber after passing through the gas absorption cell, a flow meter for measuring the gas output of the second chamber, and these pressure gauges are respectively one for measuring the gas output of the second chamber A pressure gauge for measuring the pressure value in the pipeline at the inlet end of the chamber and a pressure gauge for measuring the pressure value in the pipeline at the gas outlet end of the second chamber. By using the gas chromatograph, the flowmeters and the pressure gauges, the diffusion coefficient and permeability coefficient can be measured and calculated simultaneously.

Preferably, a solid material is assembled on the surface of the nickel plate that is in contact with the second chamber.

Preferably, the solid material is a nickel-based alloy.

The positive progressive effect of the present utility model is:

The utility model provides a hydrogen diffusion and penetration characteristic measuring device. By setting a heating system for the diffusion and permeation reactor, the measuring device can measure the diffusion and permeation characteristics of hydrogen in high-temperature molten salt and solid materials, and can also study the diffusion and permeation characteristics of hydrogen as the temperature parameters change . In addition, the measuring device can easily replace the test material, eliminate external interference and improve the test accuracy, test the diffusion characteristics and permeability characteristics of hydrogen under different temperature parameters, facilitate the control of the gas in the pipeline, stop the gas, In order to facilitate the replacement of local components, greatly improve the accuracy of the test, and simultaneously test and calculate the diffusion coefficient and permeability coefficient.

Description of drawings

FIG. 1 is a schematic structural diagram of a hydrogen diffusion and permeability measurement device in the prior art.

Fig. 2 is a structural schematic diagram of a hydrogen diffusion and permeability measurement device of the present invention.

Fig. 3 is a sectional view of the diffusion and permeation reactor of the hydrogen diffusion and permeation characteristic measuring device of the present invention.

Fig. 4 is a top view of the diffusion and permeation reactor of the hydrogen diffusion and permeation characteristic measuring device of the present invention.

Detailed ways

The preferred embodiments of the utility model are given below in conjunction with the accompanying drawings to describe the technical solution of the utility model in detail.

As shown in FIG. 2 , the device for measuring hydrogen diffusion and penetration characteristics in this embodiment is used to measure the diffusion and penetration characteristics of hydrogen in solid materials or molten salts 24 , and the solid materials mainly include stainless steel and nickel-based alloys. The device for measuring hydrogen diffusion and permeation characteristics includes a diffusion osmosis reactor 23 with a first chamber and a second chamber, a gas supply system, a measurement system and a heating system for heating the diffusion osmosis reactor 23 . In this embodiment, the first chamber and the second chamber are respectively the upper chamber 213 and the lower chamber 214 separated by the nickel plate 25 of the diffusion osmosis reactor 23 in the figure, and the heating system includes a The tubular resistance furnace 28 of the tank, the diffusion infiltration reactor is set in the heating tank.

The gas supply system includes an argon gas supply part and a hydrogen gas supply part, both of which are in communication with the upper chamber 213 and the lower chamber 214 . The argon gas supply part includes an argon gas bottle 21 , the hydrogen gas supply part includes a hydrogen gas bottle 22 , and the argon gas bottle 21 and the hydrogen gas bottle 22 communicate with the upper chamber 213 and the lower chamber 214 through valves and pipelines. The hydrogen diffusion and permeability measurement device in Fig. 2 also includes a plurality of pipelines and a plurality of valves, for example, valve V1, valve V2, valve V3, valve V4, valve V5, valve V6, valve V7, valve V8, valve V9, valve V10, valve V11, valve V12. By setting these pipeline valves, it is convenient to control the gas in the pipeline, and the gas can be stopped to facilitate the replacement of local components. FIG. 2 includes a pipeline connected between V12 and V2, which is used to test the remaining hydrogen content in the hydrogen cylinder 22 before the experiment.

The diffusion osmosis reactor 23 also includes a feeding pipeline and a molten salt adding part connected to one end of the feeding pipeline 26, and the molten salt adding part can be an existing feeding device, so it is not shown in the figure, the feeding The other end of the pipeline 26 communicates with the upper chamber 213 , and the pipeline wall of the feeding pipeline 26 is airtightly connected with the penetrating part of the first chamber. 3 and 4 clearly show the specific structure of the feeding pipeline 26 and the thermocouple 27 . In order to prevent the high temperature molten salt 24 from corroding the diffusion osmosis reactor 23, the diffusion osmosis reactor 23 is made of Monel 400 alloy to prevent gas leakage. The hydrogen diffusion and permeability measurement device also includes a vacuum suction component communicating with the upper chamber 213 and the lower chamber 214 . The vacuum suction part mainly includes a molecular pump group 29, and the molecular pump group 29 is used to evacuate the pipeline before the test, so as to reduce the influence of the residual gas in the pipeline on the measurement result. The measurement system includes a detection unit for detecting the temperature in the diffusion osmosis reactor 23 . The temperature detection component is a thermocouple 27 inserted into the high-temperature molten salt 24, and the thermocouple 27 can realize temperature measurement and control. The hydrogen diffusion and permeability measuring device also includes a gas chromatograph 212 and a HF gas absorption cell 210, the gas chromatograph 212 is connected with the HF gas absorption cell 210 through a six-way valve 211, and the six-way valve 211 is also connected with the lower chamber 214 connected. By rotating the six-way valve 211 , the gas from different pipelines can be selected to enter the gas chromatograph 212 . Therefore, the gas flowing out from the upper end of the diffusion permeation reactor 23 passes through the HF gas absorption cell 210 before entering the gas chromatograph 212 for measurement, so as to absorb the HF diffused and permeated from the molten salt 24 . After the test, the amount of tritium ions or harmful gas tritium fluoride produced under different conditions can be speculated by measuring the content of fluoride ions. The principle of the gas chromatograph 212 is to use a highly sensitive helium ionization detector to measure the amount of hydrogen diffused and infiltrated from the molten salt 24, and the detection accuracy can reach 10 ppb (1 ppb is one billionth). Therefore, the use of gas chromatograph 212 greatly improves the accuracy of the test.

The measurement system also includes four flowmeters and two pressure gauges, these flowmeters are respectively a flowmeter F1 for measuring the flow rate of argon gas supplied by the argon gas supply part, and a flowmeter F2 for measuring the flow rate of hydrogen gas supplied by the hydrogen gas supply part , a flow meter F3 for measuring the gas output of the upper chamber 213 after passing through the gas absorption pool, a flow meter F4 for measuring the gas output of the lower chamber 214, and these pressure gauges are respectively one for measuring the gas inlet of the lower chamber 214 A pressure gauge P1 for the pressure in the pipeline and a pressure gauge P2 for measuring the pressure in the pipeline at the outlet end of the lower chamber 214 . By using these flowmeters and pressure gauges, the diffusion coefficient and permeability coefficient can be measured and calculated simultaneously.

When it is necessary to measure the diffusion and permeation characteristics of hydrogen passing through the solid material, a solid material is assembled on the surface of the nickel plate 25 in contact with the lower chamber 214, and the molten salt 24 above the nickel plate 25 can be poured out.

When in use, first turn on the tube resistance furnace 28 to heat the temperature to a preset value, for example, 600°C. Close the valve V1, the valve V2, the valve V10 and the valve V11, and open all other valves, and use the molecular pump unit 29 to evacuate the system to a preset value, for example, 10 −3 Pa. Close valve V8 and valve V9, open valve V1 and valve V2, pass the mixed gas composed of a certain proportion of argon and hydrogen into the diffusion permeation reactor 23, and then pass the prepared molten salt 24 through the molten salt in a pressurized manner. Add components and feed lines 26, into the interior of the upper chamber 213. Open the valve V10 and the valve V11, turn the six-way valve 211 to communicate with the upper chamber 213, and use the gas chromatograph 212 to measure the amount of hydrogen permeated through the molten salt 24, and then turn the six-way valve 211 to communicate with the lower chamber Chamber 214, measuring the content of hydrogen in the carrier gas, so repeatedly controlling the rotation of the six-way valve 211, measuring the content of hydrogen to be measured at different times, and at the same time, recording the values of each flowmeter and pressure gauge, as well as the temperature of the thermocouple Parameters, the diffusion coefficient and permeability coefficient of hydrogen passing through the molten salt 24 at different temperatures can be calculated from these data. When it is necessary to measure the diffusion and permeation characteristics of hydrogen passing through the solid material, a solid material is also assembled on the surface of the nickel plate 25 that is in contact with the lower chamber 214, and the molten salt 24 above the nickel plate 25 is poured out and tested according to the aforementioned method That's it.

Although the specific embodiments of the present invention have been described above, those skilled in the art should understand that these are only examples, and the protection scope of the present invention is defined by the appended claims. Those skilled in the art can make various changes or modifications to these embodiments without departing from the principle and essence of the present utility model, but these changes and modifications all fall within the protection scope of the present utility model.

Claims (13)

1. hydrogen scattering and permeating characteristic measuring device; It comprises that one has scattering and permeating reactor, an air supply system and a measuring system of first chamber and second chamber; It is characterized in that this hydrogen scattering and permeating characteristic measuring device also has one and is used to the heating system that this scattering and permeating reactor heats.

2. hydrogen scattering and permeating characteristic measuring device as claimed in claim 1 is characterized in that, this heating system is one to have the tube type resistance furnace of heating tank, and this scattering and permeating reactor is arranged in this heating tank.

3. hydrogen scattering and permeating characteristic measuring device as claimed in claim 1 is characterized in that, this first chamber and this second chamber be provided with a nickel plate at the interface.

4. hydrogen scattering and permeating characteristic measuring device as claimed in claim 3; It is characterized in that; This measurement mechanism comprises that also the fused salt that a feeding tube and is connected with an end of this feeding tube adds parts; The other end of this feeding tube is connected with this first chamber, and the duct wall of this feeding tube and this airtight connection of first chamber through part.

5. hydrogen scattering and permeating characteristic measuring device as claimed in claim 1 is characterized in that, this hydrogen scattering and permeating characteristic measuring device also comprises the suction vacuum component that is connected with this first chamber and this second chamber.

6. hydrogen scattering and permeating characteristic measuring device as claimed in claim 1 is characterized in that, this measuring system comprises that one is used to detect the detection part of this scattering and permeating reactor temperature.

7. hydrogen scattering and permeating characteristic measuring device as claimed in claim 6 is characterized in that this detection part is a thermopair.

8. hydrogen scattering and permeating characteristic measuring device as claimed in claim 1; It is characterized in that; This air supply system comprises an argon gas supply part and a hydrogen supply part, and this argon gas supply part all is connected with this first chamber and this second chamber with this hydrogen supply part.

9. hydrogen scattering and permeating characteristic measuring device as claimed in claim 8; It is characterized in that; This argon gas supply part all is connected through pipeline with this first chamber and this second chamber with this hydrogen supply part; This suction vacuum component is connected through pipeline with this first chamber and this second chamber, is equipped with pipeline valve on those pipelines.

10. hydrogen scattering and permeating characteristic measuring device as claimed in claim 1; It is characterized in that; This hydrogen scattering and permeating characteristic measuring device also comprises a gas chromatograph and a HF gas absorption cell; This gas chromatograph is connected with this HF gas absorption cell to valve through one six, and this six also is connected with this second chamber to valve.

11. hydrogen scattering and permeating characteristic measuring device as claimed in claim 10; It is characterized in that; This measuring system also comprises four flowmeters and two pressure gauges; Those flowmeters be respectively one be used to measure argon gas supply part supply argon flow amount flowmeter, the flowmeter, that is used to measure hydrogen supply part supply of hydrogen flow be used to measure first chamber through gas absorption cell after the flowmeter, of air output be used to measure the flowmeter of the second chamber air output, those pressure gauges be respectively one measure the manifold pressure value of this second chamber inlet end pressure gauge and measure the pressure gauge of the manifold pressure value of this second chamber outlet side.

12. like each described hydrogen scattering and permeating characteristic measuring device of claim 1-11, it is characterized in that, this nickel plate with contacted of this second chamber on also be assembled with a solid material.

13. hydrogen scattering and permeating characteristic measuring device as claimed in claim 12 is characterized in that this solid material is a nickel-base alloy.

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