CN116413404A - Test system and test method - Google Patents
Test system and test method Download PDFInfo
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- CN116413404A CN116413404A CN202211555902.2A CN202211555902A CN116413404A CN 116413404 A CN116413404 A CN 116413404A CN 202211555902 A CN202211555902 A CN 202211555902A CN 116413404 A CN116413404 A CN 116413404A
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- 238000012360 testing method Methods 0.000 title claims abstract description 62
- 238000010998 test method Methods 0.000 title claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 241
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 157
- 239000001257 hydrogen Substances 0.000 claims abstract description 157
- 238000001035 drying Methods 0.000 claims abstract description 132
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 100
- 238000010521 absorption reaction Methods 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000002274 desiccant Substances 0.000 claims description 24
- 238000003556 assay Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 150000002431 hydrogen Chemical class 0.000 abstract description 9
- 238000004891 communication Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 229910001093 Zr alloy Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 238000005253 cladding Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
- G01N33/2025—Gaseous constituents
Abstract
The embodiment of the application provides a test system and a test method, which can be used for testing the hydrogen absorption performance of a sample. The test system comprises: a sample chamber for containing a sample; the drying device is arranged outside the sample chamber, is connected with the sample chamber and is used for receiving hydrogen and drying the hydrogen so as to supply the dried hydrogen to the sample chamber or dry the hydrogen in the sample chamber; and the detection part is connected with the sample chamber and is used for detecting the gas in the sample chamber so as to determine the hydrogen absorption condition of the sample. According to the test system and the test method provided by the embodiment of the application, the water vapor content in the hydrogen can be reduced by drying the hydrogen, so that the required water vapor concentration can be obtained, and the hydrogen with lower water content can be obtained.
Description
Technical Field
Embodiments of the present application relate to the field of testing or analyzing materials by means of determining chemical or physical properties of the materials, and in particular to a test system and a test method.
Background
Metal hydrogen absorption is a common problem in engineering that needs to be studied. Hydrogen often co-exists with water vapor, which oxidizes the metal surface and prevents hydrogen from entering the metal. Therefore, when studying the problem of hydrogen absorption by metals, it is necessary to consider the moisture content in hydrogen.
In the related art, the water content of hydrogen in the hydrogen absorption test is generally adjusted by adopting a water bath or a bubbler, and the adjustment mode determines that the hydrogen in the test has higher water content. However, in the hydrogen absorption test, the test having a lower water content in the hydrogen gas is more interesting.
Disclosure of Invention
In view of the above, embodiments of the present application provide a test system and a test method that can be used to test the hydrogen absorption properties of a sample.
According to one aspect of an embodiment of the present application, a test system includes: a sample chamber for containing a sample; the drying device is arranged outside the sample chamber, is connected with the sample chamber and is used for receiving hydrogen and drying the hydrogen so as to supply the dried hydrogen to the sample chamber or dry the hydrogen in the sample chamber; and the detection part is connected with the sample chamber and is used for detecting the gas in the sample chamber so as to determine the hydrogen absorption condition of the sample.
According to another aspect of embodiments of the present application, a test method includes: drying the hydrogen to reduce the water content in the hydrogen; supplying the dried hydrogen gas into a sample chamber in which a sample is placed; detecting the air pressure and/or the water vapor concentration in the sample chamber, and judging whether the sample absorbs hydrogen or not according to the change of the air pressure and/or the water vapor concentration.
According to yet another aspect of embodiments of the present application, a test method includes: humidifying the hydrogen to increase the water content in the hydrogen; supplying the humidified hydrogen gas into a sample chamber in which a sample is placed; the sample chamber is communicated with the drying chamber, and the drying agent in the drying chamber is utilized to adsorb the moisture in the sample chamber so as to reduce the water content in the hydrogen; and closing the sample chamber, detecting the air pressure and/or the water vapor concentration in the sample chamber, and judging whether the sample absorbs hydrogen or not according to the change of the air pressure and/or the water vapor concentration.
According to the test system and the test method, the water vapor content in the hydrogen is reduced in a manner of drying the hydrogen, so that the required water vapor concentration is obtained, and the hydrogen with lower water content can be obtained.
Drawings
The foregoing and/or additional aspects and advantages of the present application will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic diagram of a sample-containing assay system according to an embodiment of the present application;
FIG. 2 is a schematic diagram of a test system containing a sample according to another embodiment of the present application;
FIG. 3 is a schematic flow chart of a test method according to an embodiment of the present application;
FIG. 4 is a flow chart of a test method according to another embodiment of the present application.
It should be noted that the drawings are not necessarily drawn to scale and are shown only in a schematic manner that does not affect the understanding of those skilled in the art.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure. It should also be noted that, in the embodiments of the present application, the features of the embodiments and the embodiments of the present application may be combined with each other to obtain new embodiments without conflict.
The embodiment of the application provides a test system which can be used for testing the hydrogen absorption performance of a sample. In some embodiments, the sample may be a metallic material. Illustratively, the sample may be a zirconium alloy tube. After the metal absorbs hydrogen, hydrogen embrittlement or hydrogen induced cracking phenomenon can be generated, and the performance of the metal is affected. For example, zirconium alloy tubes used to house reactor fuel rods may have reduced performance after hydrogen absorption and may even compromise the operational safety of the reactor. Of course, the test system provided in the embodiments of the present application may also test any other sample capable of absorbing hydrogen, which is not limited in this application, for example, in other embodiments of the present application, the sample may be made of a non-metal material.
FIG. 1 is a schematic diagram of a sample-containing assay system according to an embodiment of the present application. As shown in fig. 1, the test system 1 may include a sample chamber 10, a drying device 20, and a detection section 30. The sample chamber 10 is for containing a sample 2. The drying device 20 is disposed outside the sample chamber 10, and the drying device 20 is connected to the sample chamber 10. The drying device 20 is configured to receive hydrogen gas and dry the hydrogen gas to supply the dried hydrogen gas to the sample chamber 10 or to dry the hydrogen gas of the sample chamber 10. The detecting section 30 is connected to the sample chamber 10 for detecting the gas in the sample chamber 10 to determine the hydrogen absorption condition of the sample 2.
The test system 1 provided in the embodiment of the present application reduces the water vapor content in the hydrogen by drying the hydrogen (i.e., the water vapor concentration in the hydrogen may be H 2 /H 2 O ratio) to obtain a hydrogen atmosphere of the desired water vapor concentration, thereby enabling hydrogen gas having a lower water content to be obtained.
The sample chamber 10 may be a sealed structure to prevent water vapor in the air from interfering with the control of the water vapor concentration in the sample chamber 10, and to facilitate the control of the air pressure in the sample chamber 10.
In some embodiments, the hydrogen gas received by the drying apparatus 20 is from a hydrogen source (e.g., a hydrogen tank). It will be readily appreciated that the hydrogen source used in industry will generally itself have a certain water content, and that the drying apparatus 20 of embodiments of the present application can obtain H by reducing the water content of the industrial hydrogen source 2 /H 2 O is greater than 5×10 3 Hydrogen (or hydrogen atmosphere) of the hydrogen absorption test is expanded 2 /H 2 The ratio of O ranges. It will be readily appreciated that hydrogen herein refers to H 2 、H 2 O-gas mixture, i.e. hydrogen with water vapor.
In an embodiment in which the hydrogen gas received by the drying apparatus 20 is from a hydrogen source (e.g., a hydrogen tank), the drying effect of the drying apparatus 20 on the hydrogen gas can be controlled by adjusting the flow rate of the gas flowing through the drying apparatus 20, thereby adjusting the concentration of water vapor in the hydrogen gas, so that the hydrogen gas having a predetermined water vapor concentration can be obtained.
In some embodiments, drying device 20 is in communication with sample chamber 10. At this time, the test hydrogen gas is already present in the sample chamber 10, and the moisture content of the hydrogen gas in the sample chamber 10 can be reduced by the drying device 20.
As shown in fig. 2, in some embodiments, the drying apparatus 20 may include a drying chamber 21 and a desiccant (not shown in fig. 2). The drying chamber 21 can communicate with the sample chamber 10. The desiccant is disposed in the drying chamber 21, and adsorbs moisture flowing into the drying chamber 21.
When hydrogen enters the drying chamber 21, moisture in the hydrogen may be adsorbed by the drying agent in the drying chamber 21. In some embodiments, the desiccant may be a solid desiccant that has a larger adsorption area that may better dry moisture in the hydrogen gas. After a period of use, the desiccant has degraded drying properties, in which case a new desiccant can be replaced.
The embodiment of the application utilizes the desiccant in the drying chamber 21 to dry the hydrogen gas, and when the hydrogen gas comes from an industrial hydrogen source, H can be obtained 2 /H 2 O is greater than 5×10 5 Hydrogen in the hydrogen absorption test is greatly expanded 2 /H 2 The ratio of O ranges.
In some embodiments, the drying apparatus 20 further comprises a drying inlet line 22, a drying outlet line 23, a first valve 24, and a second valve 25. A drying inlet line 22 is connected to the drying chamber 21 for supplying hydrogen gas to the drying chamber 21. A dry air outlet line 23 is connected between the drying chamber 21 and the sample chamber 10 to enable the drying chamber 21 to communicate with the sample chamber 10. The first valve 24 is disposed on the dry air inlet line 22, and is used for controlling the on-off of the dry air inlet line 22. The second valve 25 is disposed on the dry air outlet pipeline 23, and is used for controlling on-off of the dry air outlet pipeline 23.
In this embodiment, the dry inlet line 22 may be connected to a source of hydrogen. When the hydrogen gas received by the drying device 20 comes from the hydrogen gas source, the first valve 24 and the second valve 25 are opened, and the hydrogen gas from the hydrogen gas source flows into the drying chamber 21, is dried, and flows into the sample chamber 10.
The drying apparatus 20 may further include a flow rate adjusting valve for adjusting the flow rate of the hydrogen gas from the hydrogen gas source, i.e., adjusting the flow rate of the hydrogen gas in the drying chamber 21. The flow regulating valve may be disposed on the dry air intake line 22, and can regulate the degree of dryness of the hydrogen (i.e., regulate the water content in the hydrogen) by regulating the flow rate of the hydrogen.
When the hydrogen gas received by the drying device 20 comes from the sample chamber 10, the first valve 24 is closed and the second valve 25 is opened, and at this time, since the sample chamber 10 communicates with the drying chamber 21, the hydrogen gas in the sample chamber 10 flows between the drying chamber 21 and the sample chamber 10, and is dried in the drying chamber 21. The degree of drying of the hydrogen gas can be adjusted by controlling the duration of opening of the second valve 25.
The detection unit 30 can detect the gas in the sample chamber 10 to determine the hydrogen absorption of the sample 2. The detection unit 30 may detect the water vapor concentration, pressure, temperature, or the like in the sample chamber 10, without limitation.
As shown in fig. 2, in some embodiments, the detection portion 30 may include a moisture concentration detection portion 31. The moisture concentration detecting section 31 is configured to detect the moisture concentration in the sample chamber 10 to determine the hydrogen absorption condition of the sample 2 based on the change in the moisture concentration. When the sample 2 starts to absorb hydrogen, the moisture concentration in the sample chamber 10 increases due to the decrease in the hydrogen content, and thus, the hydrogen absorption of the sample 2 can be determined by the change in the moisture concentration. The moisture concentration detecting section 31 may be connected to the sample chamber 10 to detect the moisture concentration in the sample chamber 10.
In the case of drying the hydrogen gas by the drying device 20, the degree of drying of the hydrogen gas by the drying device 20 may be adjusted according to the moisture concentration in the sample chamber 10 detected by the moisture concentration detecting unit 31.
In the embodiment in which the hydrogen gas received by the drying device 20 is from a hydrogen gas source (such as a hydrogen tank), when the water vapor concentration in the sample chamber 10 detected by the water vapor concentration detecting portion 31 is high, the flow rate of the hydrogen gas in the drying chamber 21 can be slowed down, so that the drying effect is improved; conversely, when the water vapor concentration in the sample chamber 10 detected by the water vapor concentration detecting section 31 is low, the flow rate of hydrogen gas in the drying chamber 21 can be adjusted faster, and the drying effect is lower; when the water vapor concentration in the sample chamber 10 detected by the water vapor concentration detecting portion 31 reaches the desired concentration range, the flow rate of the hydrogen gas in the drying chamber 21 may be kept unchanged until the hydrogen gas pressure in the sample chamber 10 reaches the preset range, and the first valve 24 and the second valve 25 may be closed.
For example, in the embodiment in which the hydrogen gas received by the drying device 20 is from the sample chamber 10, when the moisture concentration in the sample chamber 10 detected by the moisture concentration detecting portion 31 is high, the second valve 25 is opened (the first valve 24 is kept closed), communication between the drying chamber 21 and the sample chamber 10 is maintained, and when the moisture concentration in the sample chamber 10 detected by the moisture concentration detecting portion 31 reaches the desired concentration range, the second valve 25 is closed.
In some embodiments, the moisture concentration detecting portion 31 may be a dew point meter capable of detecting a dew point of the gas in the sample chamber 10, from which the moisture concentration can be calculated. Dew point gauges with multiple sensors may be used to obtain a larger measurement range, for example, the dew point gauge may range from-110 deg.c to 200 deg.c. Of course, the moisture concentration detecting section 31 may be another device capable of detecting moisture concentration, such as a mass spectrometer, a chromatograph, or the like, which is not limited in this application.
As shown in fig. 2, in some embodiments, the detection portion 30 may include a barometric pressure detection portion 32. The air pressure detecting section 32 is configured to detect the air pressure in the sample chamber 10 to determine the hydrogen absorption condition of the sample 2 based on the change in the air pressure. It will be appreciated that the sealing arrangement of the sample chamber 10 allows for a certain gas pressure to be maintained in the sample chamber 10, and that as the sample 2 absorbs hydrogen, the amount of gas in the sample chamber 10 will decrease, which in turn results in a decrease in the gas pressure in the sample chamber 10. By recording the change in pressure with time, the point in time at which sample 2 starts to absorb hydrogen and the rate at which the gas pressure in sample chamber 10 decreases can be obtained, and thus the rate at which sample 2 absorbs hydrogen can be obtained. The air pressure detecting portion 32 may be connected to the sample chamber 10 to detect the air pressure in the sample chamber 10. The gas pressure detecting portion 32 may be a pressure sensor, for example, and may indicate the hydrogen pressure.
In some embodiments, the assay system 1 alsoIncluding a humidifying device 40. The humidifying device 40 is disposed outside the sample chamber 10, and the humidifying device 40 is configured to receive and humidify the hydrogen gas to supply the humidified hydrogen gas to the sample chamber 10. In the present embodiment, by providing the humidifying device 40, hydrogen gas (e.g., H) having a higher water vapor concentration can be obtained 2 /H 2 O is less than 5×10 3 ) So that sample 2 can be tested for its hydrogen absorption properties at a relatively high water vapor concentration.
In some embodiments, humidification apparatus 40 includes a bubbler 41, a humidification inlet conduit 42, a humidification outlet conduit 43, a third valve 44, and a fourth valve 45. A humidified inlet line 42 is connected to the bubbler 41 for supplying hydrogen gas to the bubbler 41. A humidified outlet line 43 is connected between the bubbler 41 and the sample chamber 10 for supplying humidified hydrogen gas to the sample chamber 10. The third valve 44 is disposed on the humidification air intake duct 42, and is used for controlling on/off of the humidification air intake duct 42. The fourth valve 45 is disposed on the humidifying air outlet pipe 43, and is used for controlling on-off of the humidifying air outlet pipe 43.
In the present embodiment, the bubbler 41 may be a device capable of passing hydrogen through water at room temperature. By setting the power of the bubbler 41, the flow rate of hydrogen, etc., the concentration of water vapor in the hydrogen gas can be adjusted. For example, hydrogen gas having a water vapor concentration of about 3% may be obtained by a bubbler.
When the humidifying device 40 is used to humidify the hydrogen gas, the third valve 44 and the fourth valve 45 may be opened simultaneously, and the hydrogen gas enters the bubbler 41 through the humidifying inlet line 42 and is humidified by the bubbler 41. The humidified hydrogen gas can enter the sample chamber 10 from the bubbler 41 through the humidified outlet line 43 for testing the hydrogen absorption performance of the sample 2.
Further, in the present embodiment, after the humidified hydrogen enters the sample chamber 10, when the water vapor concentration needs to be reduced, the drying device 20 may be used to dry the hydrogen. At this time, the first valve 24 is closed, the second valve 25 is opened, and the hydrogen gas with higher water vapor concentration in the sample chamber 10 can enter the drying chamber 21 through the drying outlet pipeline 23 and be dried by the drier in the drying chamber 21. When the hydrogen is humidified by the humidifying device 40 alone, the humidified hydrogen waterThe concentration of the vapor is generally higher, and the embodiment of the application can dry the humidified hydrogen by using the humidifying device 40 and the drying device 20 together, so that the hydrogen with a larger concentration range of the vapor can be obtained, and H in the hydrogen can be obtained 2 /H 2 O may be 10 2 ～10 5 。
In addition, when moisture from the inside of the sample chamber 10 is adsorbed by the desiccant in the drying chamber 21, it can be judged whether to stop drying the hydrogen gas (i.e., whether to close the second valve 25) based on the reading of the dew point meter. Because the space in the sample chamber 10 is relatively large, the hydrogen is relatively uniformly mixed, so that the reading of the dew point meter is relatively accurate, and the water vapor concentration of the hydrogen in the sample chamber 10 is more accurate. In other words, by connecting the sample chamber 10 and the drying chamber 21, the moisture in the hydrogen gas is statically adsorbed by the drying agent, so that the moisture concentration in the hydrogen gas can be more accurately adjusted.
In some embodiments, the assay system 1 may further comprise a gas path channel 50, the gas path channel 50 being in communication with the sample chamber 10. I.e. the gas path channel 50 is in communication with the sample chamber 10. The air passage 50 selectively communicates with the drying device 20 or the humidifying device 40. The humidifying device 40 and the drying device 20 may be connected to the air passage 50 at the same time, and the second valve 25 and the fourth valve 45 determine that the air passage 50 communicates with the drying device 20 or the humidifying device 40. For example, when the second valve 25 is closed and the fourth valve 45 is opened, the air passage 50 communicates with the humidifying device 40; when the second valve 25 is opened and the fourth valve 45 is closed, the air passage 50 communicates with the drying device 20.
As shown in fig. 2, in some embodiments, the test system 1 further includes an evacuation section 60. The evacuation section 60 is used to evacuate the sample chamber 10. The evacuation section 60 may be connected to the gas path channel 50 to effect evacuation of the sample chamber 10. The vacuumizing part 60 can degas the pipelines such as the sample chamber 10, the gas path channel and the like at the beginning of the test, so as to prevent the residual gas in the test system 1 from interfering with the test result. In some embodiments, the evacuation section 60 may be a vacuum pump. In some embodiments, the vacuum pump may include a mechanical pump and a molecular pump, which may beIn series arrangement to obtain better vacuumizing effect. Illustratively, the evacuation section 60 is capable of bringing the interior of the sample chamber 10 up to 10 -6 Vacuum degree of Pa.
In some embodiments, the test system 1 further comprises a heating portion 70. The heating section 70 is used for heating the sample 2. The heating part 70 may be disposed outside the sample chamber 10 and may be capable of heating the sample chamber 10. By providing the heating portion 70, the inside of the sample chamber 10 can be heated at the time of degassing, so that a better degassing effect can be obtained. The heating part 70 can also provide different temperatures for the sample chamber 10 to simulate the actual working condition of the sample 2 or obtain the hydrogen absorption performance of the sample 2 at different temperatures. The heating portion 70 may be an electric heating wire, a muffle furnace, or the like, and is not limited in this application.
In some embodiments, the test system 1 further comprises a hydrogen supply 80. The hydrogen supply part 80 is used to supply hydrogen to the drying device 20 or the humidifying device 40. The hydrogen supply part 80 may be connected with the dry air intake line 22 of the drying device 20 and with the humidification air intake line 42 of the humidification device 40 to supply hydrogen to the drying device 20 and the humidification device 40. The hydrogen gas in the hydrogen gas supply portion 80 may contain a certain concentration of moisture for a test of low moisture concentration. The hydrogen supply unit 80 may be a gas cylinder storing hydrogen, or a hydrogen generating device, which is not limited in this application.
Fig. 3 is a schematic flow chart of a test method according to an embodiment of the present application. As shown in fig. 3, the present embodiment also provides a test method for testing the hydrogen absorption performance of sample 2. In this embodiment, the test method may include steps S11 to S13. Specifically, in step S11, the hydrogen gas is dried to reduce the water content in the hydrogen gas. In step S12, the dried hydrogen gas is supplied into the sample chamber 10 in which the sample 2 is placed. In step S13, the air pressure and/or the water vapor concentration in the sample chamber 10 is detected, and whether the sample 2 absorbs hydrogen is determined according to the change of the air pressure and/or the water vapor concentration.
The test method provided by the embodiment can be suitable for the test of low water vapor concentration. In conducting the low moisture concentration test, the moisture concentration of the hydrogen gas used in industry is generally higher than the concentration value of the low moisture concentration test, and at this time, the moisture content in the hydrogen gas can be reduced by drying the hydrogen gas, so that the required moisture concentration can be obtained.
Whether the sample 2 absorbs hydrogen or not can be judged by the change of the air pressure alone or by the change of the water vapor concentration alone. In a preferred embodiment, it is possible to determine whether the sample 2 absorbs hydrogen by both the change in the air pressure and the change in the water vapor concentration, so that it is easier to detect that the sample 2 absorbs hydrogen.
In some embodiments, the step of drying the hydrogen gas may include: hydrogen gas is introduced into the drying chamber 21 to adsorb moisture in the hydrogen gas with a desiccant in the drying chamber 21. In the embodiment of the present application, the hydrogen is dried by the drying agent in the drying chamber 21, so that H can be obtained 2 /H 2 O is greater than 5×10 5 Hydrogen in the hydrogen absorption test is greatly expanded 2 /H 2 The ratio of O ranges.
When the drying agent in the drying chamber 21 is used to dry the hydrogen gas, the flow rate of the hydrogen gas in the drying chamber 21 (or the flow rate of the hydrogen gas flowing through the drying chamber 21) can be adjusted according to the water vapor concentration in the sample chamber 10, so that the water vapor concentration in the sample chamber 10 reaches the preset water vapor concentration range. In other words, hydrogen gas having a predetermined water vapor concentration can be obtained by adjusting the flow rate of hydrogen gas in the drying chamber 21 according to the water vapor concentration in the sample chamber 10.
For example, when the water vapor concentration in the sample chamber 10 is high, the flow rate of the hydrogen gas can be adjusted to make the adsorbent adsorb more water, thereby improving the drying effect. When the water vapor concentration in the sample chamber 10 is low, the flow rate of the hydrogen can be adjusted quickly, so that the adsorbent can absorb less water, and the drying effect is low. When the water vapor concentration in the sample chamber 10 reaches the required concentration range, the flow rate of the hydrogen can be kept unchanged; until the hydrogen gas pressure in the sample chamber 10 reaches a preset range, the supply of the dried hydrogen gas into the sample chamber 10 is stopped.
In the present embodiment, hydrogen gas may be introduced into the drying chamber 21 through the drying inlet line 22 and dried by the drying agent in the drying chamber 21. By adjusting the flow rate of hydrogen in the dry inlet line 22, the amount of moisture in the hydrogen absorbed by the desiccant can be varied, thereby achieving adjustment of the moisture concentration.
In some embodiments, the sample chamber 10 may be closed when the pressure of the dried hydrogen gas entering the sample chamber 10 reaches a preset value (the preset value should satisfy that the pressure change of the hydrogen gas in the sample chamber 10 after the hydrogen absorption can be detected). It will be readily appreciated that when the sample chamber 10 is in communication with the air path channel 50, the air path channel 50 is disconnected from the drying chamber 21, i.e., the sample chamber 10 is closed.
In some embodiments, when the sample chamber 10 is closed, it may be determined whether further drying is required based on the concentration of water vapor in the sample chamber 10. Because the hydrogen gas is more uniformly mixed in the sample chamber 10, the detected water vapor concentration is more accurate when the sample chamber 10 is closed. At this time, if the water vapor concentration is found to be high, the sample chamber 10 and the drying chamber 21 may be further connected, and the drying agent in the drying chamber 21 is used to adsorb the water in the sample chamber 10, so as to reduce the water content in the hydrogen.
The embodiment of the application also provides a test method for testing the hydrogen absorption performance of the sample 2. FIG. 4 is a flow chart of a test method according to another embodiment of the present application. In this embodiment, as shown in fig. 4, the test method may include steps S21 to S24. Specifically, in step S21, the hydrogen gas is humidified to increase the water content in the hydrogen gas. In step S22, the humidified hydrogen gas is supplied into the sample chamber 10 in which the sample 2 is placed. In step S23, the sample chamber 10 is connected to the drying chamber 21, and the drying agent in the drying chamber 21 is used to adsorb the moisture in the sample chamber 10 so as to reduce the water content in the hydrogen. In step S24, the sample chamber 10 is closed (i.e., the communication between the sample chamber 10 and the drying chamber 21 is disconnected), the air pressure and/or the water vapor concentration in the sample chamber 10 is detected, and whether the sample absorbs hydrogen is determined based on the change in the air pressure and/or the water vapor concentration.
The test method provided by the embodiment can be suitable for performing a test with high water vapor concentration. Since the water vapor concentration of industrial hydrogen gas is generally lower than the concentration value of the high water vapor concentration test when the high water vapor concentration test is performed, in this embodiment, the high water vapor concentration hydrogen gas is obtained by humidifying the hydrogen gas. After humidification of the hydrogen gas, the concentration of water vapor in the hydrogen gas is generally high (e.gH 2 /H 2 O is less than 5×10 3 ) In order to bring the water vapor concentration in the range higher than that of industrial hydrogen and lower than that of humidified hydrogen, the embodiment of the present application also specifically dries the humidified hydrogen. According to the embodiment of the application, the humidified hydrogen is dried, so that hydrogen with a larger water vapor concentration range can be obtained, and H in the hydrogen can be obtained 2 /H 2 O may be 10 2 ～10 5 。
In particular, in the embodiment of the present application, when drying, the sample chamber 10 and the drying chamber 21 are communicated, and moisture in the sample chamber 10 is adsorbed by the drying agent in the drying chamber 21. Compared with the drying mode that the hydrogen is humidified and then flows through the drying chamber 21 to be dried and then enters the sample chamber 10, the hydrogen is relatively uniformly mixed due to the relatively large space in the sample chamber 10, so that the reading of the dew point instrument is relatively accurate, and the water vapor concentration of the hydrogen in the sample chamber 10 is more accurate. In other words, by connecting the sample chamber 10 and the drying chamber 21, the moisture in the hydrogen gas is statically adsorbed by the drying agent, so that the moisture concentration in the hydrogen gas can be more accurately adjusted.
The embodiment of the application can judge whether to seal the sample chamber 10 according to the water vapor concentration in the sample chamber 10. When the moisture concentration in the sample chamber 10 is high, communication between the drying chamber 21 and the sample chamber 10 is maintained, and when the moisture concentration in the sample chamber 10 detected by the moisture concentration detecting section 31 reaches a desired concentration range, communication between the drying chamber 21 and the sample chamber 10 is interrupted.
In some embodiments, prior to detecting the air pressure and/or moisture concentration within the sample chamber 10, the test method further comprises: sample chamber 10 is heated to bring and maintain the temperature within sample chamber 10 at the test temperature.
The hydrogen absorption properties of sample 2 may be different at different temperatures. Thus, in the present embodiment, by bringing the temperature in the sample chamber 10 to and maintaining the test temperature, the hydrogen absorption performance test of the sample 2 at a predetermined temperature can be performed. In some embodiments, the predetermined temperature may be the temperature of sample 2 under actual conditions to determine the hydrogen absorption properties of sample 2 under actual conditions.
In some embodiments, the test method further comprises, prior to supplying hydrogen gas into the sample chamber 10: placing sample 2 in sample chamber 10; the sample chamber 10 is evacuated while the sample chamber 10 is heated so that the temperature of the sample chamber 10 reaches and is maintained at a pre-heat temperature, which is lower than the test temperature.
In this embodiment, the sample chamber 10 is heated while evacuating, so that the gas can be easily discharged, thereby obtaining a higher degree of vacuum. The preheating temperature is lower than the test temperature, so that the vacuum pumping is finished, and the vacuum pumping device can be heated to the test temperature more easily.
In some embodiments, multiple sets of tests at different temperatures and different water vapor concentrations may be performed in order to determine a more accurate boundary at which the sample absorbs hydrogen.
Specifically, taking a zirconium alloy cladding tube as an example, the test method of the present application is described in detail.
High water vapor concentration test: the sample chamber 10 is filled with a zirconium alloy cladding tube sample, sealed and then vacuumized by a molecular pump, and simultaneously the sample chamber 10 is heated to 150 ℃ for baking, and the vacuum degree reaches 10 -4 And stopping pumping at Pa.
Hydrogen gas was allowed to enter the sample chamber 10 through the bubbler, and when the gas pressure in the sample chamber 10 reached about 100kPa, the communication between the bubbler and the sample chamber 10 was disconnected. Sample chamber 10 and drying chamber 21 are connected, and moisture is adsorbed by the drying agent to reduce the moisture concentration in the hydrogen gas, when the dew point meter reads 5 ℃ (corresponding to H 2 /H 2 O＝1.1×10 2 ) The communication between the drying chamber 21 and the sample chamber 10 is interrupted. And continuing to heat until the temperature rises and is kept at the simulated highest practical working condition of 400 ℃, detecting the air pressure change and the water vapor concentration change of the sample chamber 10, and judging that the sample is not hydrogen-absorbed according to the pressure change, so that the zirconium alloy cladding tube is not hydrogen-absorbed under the conditions of the test temperature of 400 ℃ and the water vapor concentration.
Low water vapor concentration test: after the sample chamber 10 is re-evacuated, hydrogen gas is allowed to enter the sample chamber 10 through the drying chamber 21, and when the air pressure in the sample chamber 10 reaches about 100kPa, the communication between the drying chamber 21 and the sample chamber 10 is disconnected. At this time, the dew point meter reads at-50 ℃ and thenContinuously heating, wherein the reading of the dew point meter is changed in the heating process, and when the temperature rises and is kept at 360 ℃, the reading of the dew point meter is minus 37 ℃ and corresponds to H 2 /H 2 O＝3.3×10 3 Detecting the air pressure change and the water vapor concentration change of the sample chamber 10, judging the hydrogen absorption of the sample, and testing the result: the temperature is 360 ℃, and the water vapor concentration is H 2 /H 2 O>3.3×10 3 Is a condition for the zirconium alloy cladding tube to absorb hydrogen.
The foregoing is only examples of the present application, and is not intended to limit the scope of the patent application, and all equivalent structures or equivalent processes using the descriptions and the contents of the present application or other related technical fields are included in the scope of the patent application.
Claims (16)
1. A test system for testing hydrogen absorption properties of a sample, the test system comprising:
a sample chamber for containing the sample;
the drying device is arranged outside the sample chamber, is connected with the sample chamber and is configured to receive hydrogen and dry the hydrogen so as to supply the dried hydrogen to the sample chamber or dry the hydrogen in the sample chamber; and
and the detection part is connected with the sample chamber and is used for detecting the gas in the sample chamber so as to determine the hydrogen absorption condition of the sample.
2. The assay system of claim 1, wherein the drying apparatus comprises:
a drying chamber capable of communicating with the sample chamber; and
and the drying agent is arranged in the drying chamber and is used for adsorbing the moisture flowing into the drying chamber.
3. The assay system of claim 2, wherein the drying apparatus further comprises:
a drying air inlet pipeline connected with the drying chamber and used for supplying hydrogen to the drying chamber;
a dry air outlet pipeline connected between the drying chamber and the sample chamber so as to enable the drying chamber to be communicated with the sample chamber;
the first valve is arranged on the drying air inlet pipeline and used for controlling the on-off of the drying air inlet pipeline; and
the second valve is arranged on the drying air outlet pipeline and used for controlling the on-off of the drying air outlet pipeline.
4. The assay system of claim 1, further comprising:
the humidifying device is arranged outside the sample chamber and is used for receiving and humidifying the hydrogen so as to supply the humidified hydrogen to the sample chamber.
5. The assay system of claim 4, wherein the humidification device comprises:
a bubbler;
a humidifying inlet pipe connected to the bubbler for supplying hydrogen to the bubbler;
the humidifying and air-out pipeline is connected between the bubbler and the sample chamber and is used for supplying humidified hydrogen to the sample chamber;
the third valve is arranged on the humidifying air inlet pipeline and used for controlling the on-off of the humidifying air inlet pipeline; and
and the fourth valve is arranged on the humidifying air outlet pipeline and used for controlling the on-off of the humidifying air outlet pipeline.
6. The assay system of claim 4, further comprising:
and the air passage is communicated with the sample chamber and is selectively communicated with the drying device or the humidifying device.
7. The assay system of claim 4, further comprising:
the vacuumizing part is used for vacuumizing the sample chamber;
a heating section for heating the sample; and/or
And a hydrogen supply part for supplying hydrogen to the drying device or the humidifying device.
8. The test system according to claim 1, wherein the detection section includes:
and the water vapor concentration detection part is used for detecting the water vapor concentration in the sample chamber so as to determine the hydrogen absorption condition of the sample according to the change of the water vapor concentration.
9. The test system according to claim 1, wherein the detection section includes:
and the air pressure detection part is used for detecting the air pressure in the sample chamber so as to determine the hydrogen absorption condition of the sample according to the change of the air pressure.
10. A test method for testing hydrogen absorption properties of a sample, the test method comprising:
drying the hydrogen to reduce the water content in the hydrogen;
supplying the dried hydrogen gas into a sample chamber in which a sample is placed;
detecting the air pressure and/or the water vapor concentration in the sample chamber, and judging whether the sample absorbs hydrogen or not according to the change of the air pressure and/or the water vapor concentration.
11. The test method of claim 10, wherein drying the hydrogen gas comprises:
hydrogen is introduced into the drying chamber to adsorb moisture in the hydrogen with a desiccant in the drying chamber.
12. The assay method of claim 11, further comprising:
and adjusting the flow rate of the hydrogen in the drying chamber according to the water vapor concentration in the sample chamber.
13. A test method for testing hydrogen absorption properties of a sample, the test method comprising:
humidifying the hydrogen to increase the water content in the hydrogen;
supplying the humidified hydrogen gas into a sample chamber in which a sample is placed;
connecting the sample chamber with a drying chamber, and adsorbing the moisture in the sample chamber by using a drying agent in the drying chamber so as to reduce the water content in the hydrogen;
and closing the sample chamber, detecting the air pressure and/or the water vapor concentration in the sample chamber, and judging whether the sample absorbs hydrogen or not according to the change of the air pressure and/or the water vapor concentration.
14. The assay method of claim 13, further comprising:
and judging whether the sample chamber is closed or not according to the water vapor concentration in the sample chamber.
15. The assay of claim 10 or 13, wherein prior to detecting the air pressure and/or water vapor concentration within the sample chamber, further comprising:
the sample chamber is heated to bring and maintain the temperature within the sample chamber at the test temperature.
16. The assay method of claim 15, wherein prior to supplying hydrogen gas into the sample chamber, further comprising:
placing a sample in the sample chamber;
and vacuumizing the sample chamber, and simultaneously heating the sample chamber to enable the temperature of the sample chamber to reach and maintain at a preheating temperature, wherein the preheating temperature is lower than the test temperature.
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| CN202211555902.2A CN116413404B (en) | 2022-12-06 | Test system and test method |
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