A gas supply method and device for detecting hydrogen content in solid metal

Abstract

The present invention relates to a gas supply method and device for detecting hydrogen content in solid metals. The gas supply device is used to be connected to a hydrogen evolution chamber for hydrogen evolution in solid metals. The gas supply device mainly includes: a gas source module, a gas solenoid valve module, a gas purification module, a vacuum module and a control module. It can provide carrier gas for sample hydrogen content detection and hydrogen-containing calibration gas for high-temperature hydrogen sensor calibration. The gas supply process matches the test process, has a high degree of automation and high detection efficiency; and meets the calibration requirements of different hydrogen concentrations, improving the accuracy of gas flow control.

Description

Technical Field

[0001] The present invention relates to the technical field of detecting the content of substances in samples, and more particularly to detecting the content of hydrogen in solid metal samples, such as detecting the content of diffused hydrogen or total hydrogen in steel blocks, aluminum blocks, and metal welded joints, and more particularly to a gas supply method and device for detecting the content of hydrogen in solid metals. Background Art

[0002] Hydrogen sensors made with functional ceramics as core components are a type of high-temperature sensor that has developed rapidly in recent years. This sensor has gradually been used to detect hydrogen content in high-temperature media such as liquid metals and molten salts. Depending on the type of material, the high temperature at which various materials precipitate hydrogen is different. For the detection of hydrogen content in solid metals, if a high-temperature hydrogen sensor is used, the hydrogen precipitated at high temperature (generally 300-500°C or higher) can be directly detected without cooling and secondary collection of hydrogen. Compared with traditional thermal conductivity cells, gas chromatographs and infrared element detection modules, the use of high-temperature hydrogen sensors can realize high-temperature in-situ testing of hydrogen content in solid metals without the need for secondary collection of hydrogen. The hydrogen measurement device using this method is smaller and more portable, has higher hydrogen measurement efficiency and is relatively cheaper. When using a high-temperature hydrogen sensor to detect hydrogen content in solid metals, a gas supply device is required to provide carrier gas to the hydrogen evolution chamber for gas replacement and purge in the hydrogen evolution chamber or to provide carrier gas during the hydrogen evolution process; during the calibration process of the hydrogen measurement device, a gas supply device is required to provide the hydrogen measurement device with calibration gas with a known hydrogen content to calibrate the hydrogen measurement device. As an important module of the hydrogen content detection device in solid metal, the gas supply device plays an important role in the detection of hydrogen content and the calibration of the hydrogen measurement device. However, the current gas supply device has a single gas supply method and a low degree of automation, which makes the detection efficiency low and the data has large errors, seriously affecting the detection results. Summary of the invention

[0003] In view of the deficiencies in the prior art, the present invention provides a gas supply method and device for detecting the hydrogen content in solid metals, which can provide carrier gas for detecting the hydrogen content of solid metal samples and provide hydrogen-containing calibration gas for calibrating a high-temperature hydrogen sensor in a detection device. The gas supply process matches the test process, has a high degree of automation, and has high detection efficiency. In addition, high-hydrogen concentration calibration gas or low-hydrogen concentration calibration gas is provided to meet the calibration requirements of different hydrogen concentrations, realize the calibration of high-temperature hydrogen sensors, avoid the influence of the sensor's own factors on the accuracy of metal hydrogen content detection, and improve the detection accuracy of data. At the same time, by selecting a large-flow gas flow controller and a small-flow gas flow controller, the requirements of different gas flow rates entering a hydrogen evolution chamber can be met, the gas flow control accuracy can be improved, and the accuracy of the calibration process and solid metal hydrogen content detection data can be further improved.

[0004] In order to solve at least one of the above technical problems, the technical solution adopted by the present invention is:

[0005] On the one hand, the present invention provides a gas supply device for detecting hydrogen content in solid metal, characterized in that the gas supply device is used to be connected to a hydrogen evolution chamber for hydrogen evolution of solid metal, and the gas supply device comprises:

[0006] A gas source module, the gas source module comprising a hydrogen-containing calibration gas source and a carrier gas source;

[0007] A gas solenoid valve module, the gas solenoid valve module comprising: a carrier gas solenoid valve, a hydrogen-containing calibration gas solenoid valve, a first gas solenoid valve, a second gas solenoid valve and a gas outlet solenoid valve, wherein the carrier gas solenoid valve is connected to the carrier gas source, and the hydrogen-containing calibration gas solenoid valve is connected to the hydrogen-containing calibration gas source;

[0008] A gas purification module, wherein the inlet of the gas purification module is connected to the carrier gas solenoid valve and the hydrogen-containing calibration gas solenoid valve respectively, the outlet of the gas purification module is connected to the inlet of the first gas solenoid valve via a first gas flow controller, the outlet of the first gas solenoid valve is connected to the gas inlet of the sample pre-release area of ​​the hydrogen evolution chamber, and the outlet of the gas purification module is connected to the inlet of the second gas flow controller via the second gas solenoid valve, and the outlet of the second gas flow controller is connected to the gas inlet of the heating area of ​​the hydrogen evolution chamber;

[0009] A vacuum pumping module, wherein the vacuum pumping module is connected to the gas outlet of the heating zone of the hydrogen evolution chamber via the gas outlet solenoid valve;

[0010] A control module is used for the overall operation of the air supply device.

[0011] Furthermore, it also includes: a pressure reducing valve module, the carrier gas solenoid valve is connected to the carrier gas source via the pressure reducing valve module, and the hydrogen-containing calibration gas solenoid valve is connected to the hydrogen-containing calibration gas source via the pressure reducing valve module.

[0012] Furthermore, it also includes: a pressure display module, which includes: a gas source pressure gauge and a hydrogen evolution chamber pressure gauge, the gas source pressure gauge is arranged at the inlet of the gas purification module, and the hydrogen evolution chamber pressure gauge is arranged at the gas inlet of the heating zone of the hydrogen evolution chamber.

[0013] Furthermore, the gas purification module includes: a water vapor removal unit and a carbon dioxide removal unit, the inlet of the water vapor removal unit is respectively connected to the carrier gas solenoid valve and the hydrogen-containing calibration gas solenoid valve, the inlet of the carbon dioxide removal unit is connected to the outlet of the water vapor removal unit, and the outlet of the carbon dioxide removal unit is respectively connected to the first gas flow controller and the second gas solenoid valve.

[0014] Furthermore, a high-temperature hydrogen sensor for detecting the concentration of hydrogen precipitated from the solid metal is provided in the heating zone.

[0015] Furthermore, the hydrogen-containing calibration gas source includes: a high hydrogen concentration calibration gas source with a volume fraction of 10% and a low hydrogen concentration calibration gas source with a volume fraction of 0.1%.

[0016] Furthermore, the carrier gas stored in the carrier gas source includes nitrogen or an inert gas, and the hydrogen-containing calibration gas stored in the hydrogen-containing calibration gas source is a hydrogen-inert gas mixture, preferably a hydrogen-argon mixture.

[0017] Furthermore, the control module is a PLC, an industrial control computer or a personal computer.

[0018] On the other hand, the present invention provides a gas supply method for detecting the hydrogen content in solid metal using the gas supply device, characterized in that it comprises the following steps:

[0019] S1: Close the hydrogen-containing calibration gas solenoid valve through the control module, open the carrier gas solenoid valve, and adjust the pressure reducing valve module to make the pressure reach slightly greater than one atmosphere;

[0020] S2: placing the solid metal sample in the sample pre-placement area of ​​the hydrogen evolution chamber, closing the first gas solenoid valve and the second gas solenoid valve, opening the gas outlet solenoid valve at the same time, setting the first gas flow controller to a certain gas flow rate, and then controlling the vacuum pumping module to vacuum the hydrogen evolution chamber, closing the gas outlet solenoid valve and the vacuum pumping module to put the hydrogen evolution chamber in a vacuum state;

[0021] S3: Open the first gas solenoid valve to allow the carrier gas in the carrier gas source to flow into the hydrogen evolution chamber through the first gas solenoid valve. When the pressure in the hydrogen evolution chamber is greater than one atmosphere, open the gas outlet solenoid valve to allow the carrier gas to continuously purge the solid metal sample and the hydrogen evolution chamber and replace the hydrogen evolution chamber with a carrier gas atmosphere.

[0022] S4: moving the solid metal sample into the heating zone of the hydrogen evolution chamber, opening the second gas solenoid valve, and closing the first gas solenoid valve, adjusting the second gas flow controller to allow the carrier gas to flow in the hydrogen evolution chamber, and in the process of heating the solid metal sample to precipitate hydrogen, the carrier gas gradually carries the precipitated hydrogen out of the hydrogen evolution chamber through the gas outlet solenoid valve;

[0023] S5: After all the hydrogen in the solid metal sample is precipitated, the second gas solenoid valve is closed, and then the first gas solenoid valve is opened to continuously purge and cool the interior of the hydrogen evolution chamber with the carrier gas.

[0024] On the other hand, the present invention provides a gas supply method for calibrating a high-temperature hydrogen sensor using the gas supply device, characterized in that it comprises the following steps:

[0025] S1: Open the hydrogen-containing calibration gas solenoid valve through the control module, close the carrier gas solenoid valve, and adjust the pressure reducing valve module to make the pressure reach slightly greater than one atmosphere;

[0026] S2: close the first gas solenoid valve and the second gas solenoid valve, open the gas outlet solenoid valve at the same time, set the first gas flow controller to reach a certain gas flow rate, control the vacuum module to vacuum the hydrogen evolution chamber, close the gas outlet solenoid valve and the vacuum module, and put the hydrogen evolution chamber in a vacuum state;

[0027] S3: Open the first gas solenoid valve to allow the hydrogen-containing calibration gas in the hydrogen-containing calibration gas source to flow into the hydrogen evolution chamber through the first gas solenoid valve. When the pressure in the hydrogen evolution chamber is greater than one atmosphere, open the gas outlet solenoid valve to allow the hydrogen-containing calibration gas to continuously purge the hydrogen evolution chamber and replace the hydrogen evolution chamber with the hydrogen-containing calibration gas atmosphere.

[0028] S4: Open the second gas solenoid valve and close the first gas solenoid valve, adjust the second gas flow controller to make the hydrogen-containing calibration gas flow in the hydrogen evolution chamber, and when the temperature inside the hydrogen evolution chamber reaches the test temperature of the high-temperature hydrogen sensor, the high-temperature hydrogen sensor detects the hydrogen concentration in the hydrogen evolution chamber, and compares the detection result with the actual hydrogen concentration of the hydrogen-containing calibration gas to achieve calibration of the high-temperature hydrogen sensor.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] (1) A high-temperature hydrogen sensor that can be used directly at high temperatures is used as a hydrogen measuring element, so that the precipitation and detection of hydrogen in solid metals can be carried out simultaneously. There is no need to collect the precipitated hydrogen and then detect the hydrogen content. This design makes the device more portable and simple;

[0031] (2) A structural form in which a cylinder branch is provided on the cylinder, and a sample pre-placement area and a heating area are set for the hydrogen evolution chamber. Before heating and hydrogen evolution, the metal sample to be tested is temporarily placed in the sample pre-placement area and fully purged by the carrier gas, which can greatly reduce the interference of the adsorbed gas on the sample surface on the hydrogen content detection result;

[0032] (3) The cooling element can quickly cool the hydrogen evolution chamber, speed up sample analysis time, and improve test efficiency;

[0033] (4) By adding blank tests, the influence of the detection device itself on the accuracy of metal hydrogen content detection is reduced, and the detection accuracy of the data is improved;

[0034] (5) The gas supply device can provide carrier gas for the detection of hydrogen content in solid metal samples, and can also provide hydrogen-containing calibration gas for the calibration of high-temperature hydrogen sensors in the detection device. The gas supply process matches the test process, and the degree of automation is high;

[0035] (6) It can provide high hydrogen concentration calibration gas or low hydrogen concentration calibration gas to meet the calibration requirements of different hydrogen concentrations, realize the calibration of high temperature hydrogen sensors, avoid the influence of sensor's own factors on the accuracy of metal hydrogen content detection, and improve the detection accuracy of data;

[0036] (7) By selecting a large-flow gas flow controller and a small-flow gas flow controller, the requirements of different gas flow rates entering the hydrogen evolution chamber can be met, the accuracy of gas flow control can be improved, and the accuracy of the calibration process and solid metal hydrogen content detection data can be further improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 This is a structural block diagram of the detection device of the present invention.

[0038] Figure 2 It is a schematic diagram of the structure of the hydrogen evolution chamber of the present invention.

[0039] Figure 3 This is a schematic diagram of placing the solid metal sample of the present invention.

[0040] Figure 4 This is a flow chart of the blank test of hydrogen content in the present invention.

[0041] Figure 5 This is a flow chart of solid metal hydrogen content detection in the present invention.

[0042] Figure 6 It is the hydrogen concentration-time distribution curve.

[0043] Figure 7 The figure is a schematic diagram of the structure of an air supply device according to an embodiment of the present invention.

[0044] Figure 8 The present invention is a control principle block diagram of a control module in an air supply device according to an embodiment of the present invention.

[0045] In the above figures: 1-cylinder; 2-first cylinder end cap; 3-second cylinder end cap; 4-cylinder branch end cap; 5-temperature sensor; 6-high-temperature hydrogen sensor; 7-solid metal sample; 8-heating element; 9-cooling element; 100-gas supply unit; 101-sample pre-release area; 102-heating area; 103-cylinder branch; 104-push rod; 11-heating area gas inlet; 12-heating area gas outlet; 13-cylinder sealing element 1; 14-cylinder sealing element 2; 15-sample pre-release area gas inlet; 16-cylinder branch sealing element; 17-sample push rod channel; 18-temperature sensor sensing element; 19-high-temperature hydrogen sensor sensing element; 20-vacuum pump; 21-hydrogen concentration-time curve; 22-geometric area enclosed by the curve and the time coordinate axis; 231-carrier gas source; 232-high hydrogen concentration Calibration gas source; 233-low hydrogen concentration calibration gas source; 241-first pressure reducing valve; 242-second pressure reducing valve; 243-third pressure reducing valve; 251-carrier gas solenoid valve; 252-first hydrogen-containing calibration gas solenoid valve; 253-second hydrogen-containing calibration gas solenoid valve; 261-first gas source pressure gauge; 262-second gas source pressure gauge; 271-water vapor removal unit; 272-carbon dioxide removal unit; 281-first gas flow controller; 282-first gas solenoid valve; 291-large flow gas solenoid valve; 292-large flow gas flow controller; 293-small flow gas solenoid valve; 294-small flow gas flow controller; 30-hydrogen evolution chamber pressure gauge; 31-processor; 32-signal conversion module; 33-switch input and output module; 34-analog input module; 35-gas outlet solenoid valve; 36-hydrogen evolution chamber. DETAILED DESCRIPTION

[0046] In order to make those skilled in the art better understand the technical scheme of the present invention, the present invention is further described in detail below in conjunction with specific embodiments. The embodiments described below are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention. If no specific technology or conditions are specified in the embodiments, the technology or conditions described in the literature in this area or the product specification are used.

[0047] Embodiment 1: According to this embodiment of the present invention, a device for detecting hydrogen content in solid metal is provided. Figure 1 It is a structural block diagram of the detection device of the present invention, such as Figure 1 As shown, the device mainly includes: a gas supply control unit, a gas supply unit, a hydrogen evolution chamber, a signal acquisition unit, a temperature control unit and a control processing system.

[0048] During the test, the solid metal sample is placed in the hydrogen evolution chamber, and the gas supply unit is connected to the hydrogen evolution chamber to provide the hydrogen evolution chamber with a carrier gas for purging the solid metal sample before heating and as a carrier gas for hydrogen during the hydrogen evolution process. The gas supply control unit and the gas supply unit together constitute a gas supply device, and the gas supply control unit is connected to the gas supply unit to control the gas supply unit. Specifically, the gas supply control unit is used to control the on and off of the relevant valves in the gas supply unit, set the flow of the gas flow control element, and obtain the gas pressure signal in the gas supply unit.

[0049] In this embodiment of the present invention, the specific type of the gas supply device (gas supply control unit and gas supply unit) is not particularly limited as long as gas supply can be achieved.

[0050] According to this embodiment of the present invention, the carrier gas should be nitrogen or an inert gas that does not react with hydrogen and solid metal.

[0051] It can be understood that the sensing elements of the high-temperature hydrogen sensor and the temperature sensor of the present invention are arranged inside the hydrogen evolution chamber, specifically in the heating zone of the hydrogen evolution chamber.

[0052] The signal acquisition unit is connected to the high-temperature hydrogen sensor and the temperature sensor respectively, and is used to acquire electrical signal data of the high-temperature hydrogen sensor and the electrical signal data of the temperature sensor.

[0053] According to this embodiment of the present invention, the specific type of the signal acquisition unit is not particularly limited, as long as it can realize signal acquisition, such as a commonly used signal acquisition instrument or a related signal acquisition sensor.

[0054] The temperature control unit is used to control the internal temperature of the hydrogen evolution chamber, and is composed of a heating element and a cooling element. The heating element can control the temperature rise process inside the hydrogen evolution chamber to indirectly control the hydrogen precipitation process in the solid metal sample. The cooling element can be used to control the temperature drop process inside the hydrogen evolution chamber to prepare for the next sample test after the test of one sample is completed, thereby improving the test efficiency.

[0055] According to this embodiment of the present invention, the heating element may be a resistance wire, a heating carbon rod, a silicon molybdenum rod, a microwave heating element or an infrared heating element, or other types of heating devices; the cooling element may be a fan, a cooler or other cooling equipment. In this embodiment, the temperature control scheme is preferably a "proportional-integral-differential" control scheme, which is a conventional technology and is not described in detail here.

[0056] In this embodiment of the present invention, the specific type of the control processing system is not limited, and can be a PLC, an industrial control computer, a personal computer or an embedded processor, or other systems that can achieve the same functions. This embodiment is preferably a PLC control processing system.

[0057] More specifically, the control and processing system includes an electrical control unit, a signal acquisition unit and a processing unit. The electrical control unit of the control and processing system is connected to the gas supply control unit and the temperature control unit respectively, and the signal acquisition unit is connected to the signal acquisition unit, and is used to control and acquire data from the relevant units, specifically: controlling the on and off of the relevant solenoid valves in the gas supply control unit to achieve the control of the gas flow rate and the flow rate, thereby controlling the gas supply process; through the data detected by the temperature sensor, the electrical control unit accurately controls the temperature control unit to achieve the control of the temperature in the hydrogen evolution chamber; the signal acquisition unit communicates with the signal acquisition unit through a serial port or parallel port communication method to indirectly acquire the detection data of the digital high-temperature hydrogen sensor and the temperature sensor; the processing unit is connected to the electrical control unit and the signal acquisition unit respectively, and analyzes the collected carrier gas flow rate and hydrogen concentration data to calculate the hydrogen content in the solid metal, more specifically: according to the real-time hydrogen concentration C(t) and the carrier gas flow rate v in the hydrogen evolution chamber continuously acquired, the hydrogen content in the solid metal is obtained by integrating the process within a certain hydrogen evolution time, including: the hydrogen evolution time is t 开始 The end time of hydrogen evolution is t 结束 , then the hydrogen content of the solid metal released during the hydrogen evolution process is

[0058] Figure 2 Schematic diagram of the structure of the hydrogen evolution chamber of the present invention. Figure 3 This is a schematic diagram of placing the solid metal sample of the present invention, as shown in Figure 2 and 3 As shown, the hydrogen evolution chamber 36 of the present invention is mainly composed of the following parts: a cylinder 1, a cylinder branch 103, a first cylinder end cap 2, a second cylinder end cap 3, a cylinder branch end cap 4, a sample pre-release area 101, a heating area 102, a cylinder sealing element 13, a cylinder sealing element 2 14, and a cylinder branch sealing element 16. Among them, the cylinder branch 103 is vertically installed on the cylinder 1 and is an integrally connected structure with the cylinder 1, the first cylinder end cap 2 and the second cylinder end cap 3 are installed at both ends of the cylinder 1, and the cylinder branch end cap 4 is installed at the end of the cylinder branch 103. The installation method is threaded installation, and it can also be other detachable installation methods. The shape of the cylinder and the cylinder branch is not limited. This embodiment of the present invention is preferably cylindrical, which is convenient for processing and manufacturing and uniform heating of the heating area. The internal space of the cylinder 1 is the heating area 102, and the internal space of the cylinder branch is the sample pre-release area 101. A cylinder sealing element 13 and a cylinder sealing element 2 14 are respectively installed between the first cylinder end cover 2, the second cylinder end cover 3 and the cylinder 1, and a cylinder branch sealing element 16 is installed between the cylinder branch end cover 4 and the cylinder branch 103. It can be understood that all sealing elements are used to prevent gas leakage from the hydrogen evolution chamber, and the specific types are not limited. In this embodiment, a high temperature resistant sealing ring or a sealing gasket is preferably used.

[0059] Continue to refer to Figure 2 and 3 As shown, a heating zone gas inlet 11 is provided on the first cylinder end cover 2, which is connected to the gas supply unit 100 to provide carrier gas for purging and hydrogen carrier for the hydrogen evolution chamber. The temperature sensor 5 and the high-temperature hydrogen sensor 6 are simultaneously installed and fixed on the first cylinder end cover 2, and the temperature sensor sensing element 18 and the high-temperature hydrogen sensor sensing element 19 are located in the heating zone 102 of the hydrogen evolution chamber, respectively used to measure the temperature of the heating zone and the hydrogen concentration in the hydrogen evolution chamber. A heating zone gas outlet 12 is provided on the second cylinder end cover 3 for discharging gas in the hydrogen evolution chamber. The cylinder branch end cover 4 is provided with a sample pre-discharge zone gas inlet 15 and a sample push rod channel 17. The sample pre-discharge zone gas inlet 15 is connected to the gas supply unit 100 to provide a purge carrier gas for the sample pre-discharge zone and the heating zone. The sample push rod channel 17 is used for the operator to extend the push rod 104 from the outside to the inside into the sample pre-discharge zone 101, and push the solid metal sample to be tested from the sample pre-discharge zone 101 to the heating zone 102 for the subsequent heating and hydrogen evolution process.

[0060] According to some embodiments of the present invention, a through valve is installed outside the sample push rod channel 17 , and the through valve can be opened when pushing the sample, so that the push rod 104 can push the solid metal sample 7 through the sample push rod channel 17 .

[0061] The heating element 8 is placed outside the cylinder 1 where the heating zone 102 is located, and is used to heat the solid metal sample 7 in the heating zone 102 to precipitate hydrogen in the sample at high temperature. The cooling element 9 is arranged near the heating element 8, and is used to quickly cool down the heating zone after the sample test is completed, so as to prepare for the next sample test process and improve the test efficiency.

[0062] Embodiment 2: According to this embodiment of the present invention, a detection method using the hydrogen content detection device in solid metal described in the aforementioned embodiment 1 is provided. When the hydrogen content is detected, the solid metal sample 7 is first placed in the sample pre-discharge area 101 of the hydrogen evolution chamber, and the temperature and hydrogen concentration in the hydrogen evolution chamber are detected by the temperature sensor 5 and the high-temperature hydrogen sensor 6. The carrier gas is provided to the sample prevention area 101 and the heating area 102 of the hydrogen evolution chamber by the gas supply unit 100. The carrier gas is selected as nitrogen or an inert gas that does not react with hydrogen and solid metal. Before measuring hydrogen, the air in the hydrogen evolution chamber needs to be exhausted. Before the carrier gas is introduced, the hydrogen evolution chamber can be evacuated by the vacuum pump 20 outside the hydrogen evolution chamber, and then the carrier gas is introduced to achieve rapid replacement of the gas in the hydrogen evolution chamber.

[0063] In order to reduce the impact of the detection device's own factors on the accuracy of hydrogen content detection in metals, at least one hydrogen content blank test is required before starting the hydrogen content test (that is, no solid metal sample is placed and the detection device itself is tested), and then subsequent solid metal hydrogen content tests are carried out, which is beneficial to improve the accuracy of the test data.

[0064] Figure 4 This is a flow chart of the blank test of hydrogen content in the present invention, as shown in Figure 4 As shown, the blank test process mainly includes: gas replacement (specifically including: evacuating the hydrogen evolution chamber by a vacuum pump, and then introducing a high-purity carrier gas to replace the original air in the hydrogen evolution chamber with a high-purity carrier gas atmosphere); then continuing to introduce the high-purity carrier gas at a certain flow rate; then heating the hydrogen evolution chamber to reach the hydrogen evolution temperature, and the process continuously measures the hydrogen concentration C0(t) in the hydrogen evolution chamber by a high-temperature hydrogen sensor, and the real-time hydrogen concentration C0(t) is in ppm, that is, the volume of hydrogen in every 1 million milliliters of gas in the hydrogen evolution chamber; after a certain period of high-temperature heating, when the detected hydrogen concentration is zero and no longer changes, the control processing system calculates the hydrogen content according to the obtained carrier gas flow rate and the continuously collected hydrogen concentration data, and obtains the hydrogen content q0 in milliliters during the blank test; then the hydrogen evolution chamber is purged and cooled with a large flow rate by the carrier gas, and the cooling element cools the hydrogen evolution chamber from the outside, and the blank test process is ended.

[0065] Figure 5 This is a flow chart of solid metal hydrogen content detection in the present invention, as shown in Figure 5As shown in the figure, the detection process of hydrogen content in solid metal is mainly as follows: prepare the solid metal sample to be tested, so that its surface is free of impurities such as oil, moisture, etc. For the long strip metal sample, its size is not more than 10mm×10mm×40mm, and for the cylindrical sample, its diameter should be not more than 10mm and the length is not more than 40mm; weigh the sample to obtain its mass m in grams; pre-place the sample in the sample prevention area of ​​the hydrogen evolution chamber; perform gas replacement (specifically including: vacuum pumping the hydrogen evolution chamber, then introducing high-purity carrier gas, and replacing the original air inside the hydrogen evolution chamber with high-purity carrier gas atmosphere); then continue to introduce high-purity carrier gas at a certain flow rate; then move the sample from the sample prevention area to the heating area; start the signal acquisition unit and the high-temperature hydrogen sensor to start continuously acquiring the real-time hydrogen concentration C1(t) in the hydrogen evolution chamber, and the data acquisition frequency is not less than 10 times / second, and send the continuously acquired data to the control processing system, and then control the heating element to heat the hydrogen evolution chamber to achieve hydrogen evolution. The temperature is set, and the hydrogen content is precipitated into the hydrogen precipitation chamber. The real-time hydrogen concentration C1(t) is in ppm, i.e., the volume of hydrogen in the gas in the hydrogen precipitation chamber per 1 million milliliters. After a certain period of time, when all the hydrogen in the solid metal is released, the hydrogen concentration detected by the high-temperature hydrogen sensor drops to zero and no longer changes. At this time, the control and processing system calculates the hydrogen content precipitated in this test according to the carrier gas flow rate obtained in the hydrogen precipitation process and the hydrogen concentration data obtained continuously, and obtains the hydrogen content q1 in milliliters. The actual total hydrogen content q (q=q1-q0) in the solid sample is obtained by subtracting q0 from q1, and the unit is milliliters. The hydrogen concentration in the metal to be tested is finally obtained as Q=100*q / m, i.e., the hydrogen content contained in every 100 grams of solid metal, which is used as a judgment index of the hydrogen content in the solid metal. After the test is completed, a relatively large flow rate carrier gas is introduced to purge and cool the hydrogen precipitation chamber, and the external cooling element of the hydrogen precipitation chamber also cools the hydrogen precipitation chamber. After cooling to a temperature below 100° C., the sample is taken out to terminate the hydrogen measurement.

[0066] In this embodiment of the present invention, the purity of the high-purity carrier gas should be no less than 99.99% by volume.

[0067] Figure 6 The hydrogen concentration-time distribution curve is shown in Figure 2. During the blank test and the detection of hydrogen content in solid metal, the hydrogen content q0 and q1 are calculated based on the hydrogen concentration C(t) in the hydrogen evolution chamber continuously obtained by the sensor. Figure 6 As shown, it includes: drawing a continuous curve of the hydrogen content measured by the high-temperature hydrogen sensor during the blank test and the detection of hydrogen content in the solid metal against time, and the curve records the real-time hydrogen concentration C(t) in the hydrogen evolution chamber from the start of heating to the start of hydrogen evolution, to the end of hydrogen evolution and the end of heating. Assume that the flow rate of the flowing carrier gas through the hydrogen evolution chamber during the hydrogen evolution process is constant at v, in milliliters per second, and the start time of hydrogen evolution is t 开始 The end time of hydrogen evolution is t结束 , then the hydrogen content released in the total hydrogen evolution process is That is, the geometric area 22 enclosed by the hydrogen concentration-time curve 21 and the time coordinate axis is With v×10 -6 The method can be used to calculate the hydrogen content q0 in the blank test and the hydrogen content q1 in the solid metal hydrogen content test, and the difference between the two is the actual hydrogen content in the metal. More specifically, when the hydrogen content in the solid metal is detected: according to the real-time hydrogen concentration C1(t) and the flow rate v1 of the carrier gas, the hydrogen content in the solid metal is obtained by integrating the hydrogen evolution time, including: the start time of hydrogen evolution is t1 / s, the end time of hydrogen evolution is t2 / s, and the hydrogen content q1 released during the hydrogen evolution process is Similarly, during the blank test: according to the real-time hydrogen concentration C0(t) and the flow rate v0 of the carrier gas, the hydrogen content in the hydrogen evolution chamber is obtained by integration processing during the hydrogen evolution time, including: the start time of hydrogen evolution is t3 / s, the end time of hydrogen evolution is t4 / s, and the hydrogen content q0 released during the hydrogen evolution process is This is the hydrogen content during blank detection. Subtract q0 from q1 to get the actual total hydrogen content q in the solid sample (q = q1 - q0), in milliliters.

[0068] Embodiment 3: According to this embodiment of the present invention, a gas supply device for detecting the hydrogen content in solid metals in the aforementioned embodiments 1 and 2 is provided. The gas supply device provided in this embodiment can provide carrier gas for detecting the hydrogen content of solid metal samples, and can also provide hydrogen-containing calibration gas for calibrating the detection device. The gas supply process matches the test process, and the degree of automation is high. High hydrogen concentration calibration gas or low hydrogen concentration calibration gas can be provided to meet the calibration requirements of different hydrogen concentrations, realize the calibration of high-temperature hydrogen sensors, avoid the influence of the sensor's own factors on the accuracy of metal hydrogen content detection, and improve the detection accuracy of the data. By selecting a large-flow gas flow controller and a small-flow gas flow controller, the requirements of different gas flow rates entering the hydrogen evolution chamber can be met, the accuracy of gas flow control can be improved, and the accuracy of the calibration process and solid metal hydrogen content detection data can be further improved.

[0069] Figure 7 FIG. 1 is a schematic diagram of the structure of the gas supply device of this embodiment of the present invention, as shown in FIG. Figure 7 As shown, the gas supply device provided by the present invention is a part of the hydrogen content detection device in solid metal of Example 1, and is used to provide gas to the hydrogen evolution chamber. The gas supply device of this embodiment mainly includes eight modules: a gas source module, a pressure reducing valve module, a gas solenoid valve module, a pressure display module, a gas purification module, a flow control module, a vacuum module and a control module.

[0070] In this embodiment, the gas source module includes a carrier gas source 231, a high hydrogen concentration calibration gas source 232 and a low hydrogen concentration calibration gas source 233. The carrier gas is a gas that does not react with the solid metal to be measured and hydrogen, preferably an inert gas such as nitrogen or argon. One bottle of hydrogen-containing calibration gas is a high hydrogen concentration mixed gas, specifically: hydrogen-inert gas mixed gas, preferably hydrogen-argon mixed gas, such as a hydrogen-argon mixed gas with a volume fraction of 10%. The other bottle of hydrogen-containing calibration gas is a low hydrogen concentration mixed gas, specifically: hydrogen-inert gas mixed gas, preferably hydrogen-argon mixed gas, such as a hydrogen-argon mixed gas with a volume fraction of 0.1%. It can be understood that the gas source described in the present invention is a gas storage container, the specific type is not limited, and this embodiment preferably uses a vertical gas cylinder.

[0071] In this embodiment, the pressure reducing valve module includes three pressure reducing valves matched with the gas source, specifically: a first pressure reducing valve 241, a second pressure reducing valve 242 and a third pressure reducing valve 243, which are used to control the output gas pressure of the gas source module.

[0072] In this embodiment, the gas solenoid valve module includes a carrier gas solenoid valve 251, a first hydrogen-containing calibration gas solenoid valve 252, a second hydrogen-containing calibration gas solenoid valve 253, a first gas solenoid valve 282, a second gas solenoid valve and a gas outlet solenoid valve 35, and the second gas solenoid valve includes: a large flow gas solenoid valve 291 and a small flow gas solenoid valve 293, which are used to control the flow or cutoff of gas in the gas supply device.

[0073] In this embodiment, the pressure display module includes a first gas source pressure gauge 261, a second gas source pressure gauge 262 and a hydrogen evolution chamber pressure gauge 30, wherein the first gas source pressure gauge and the hydrogen evolution chamber pressure gauge are electronic pressure gauges that can output pressure signals to the control module, and the gas source pressure gauge 2 is a dial display type pressure gauge that can be directly observed.

[0074] In this embodiment, the gas purification module includes a water vapor removal unit 271 and a carbon dioxide removal unit 272. It can be understood that the water vapor removal unit and the carbon dioxide removal unit can remove water vapor and carbon dioxide respectively. The specific treatment measures are not particularly limited and are conventional technologies and are not described in detail here.

[0075] In this embodiment, the flow control module includes a first gas flow controller 281 and a second gas flow controller, the first gas flow controller is used to control the displacement purge rate of the carrier gas or the hydrogen-containing calibration gas to the air before the hydrogen measurement heating in the hydrogen analysis chamber, the purge rate of the carrier gas to the solid metal sample before the hydrogen measurement heating, and the cooling rate of the hydrogen analysis chamber after the sample test is completed. It can be understood that the larger the flow rate, the faster the corresponding purge speed, and the faster the cooling speed of the hydrogen analysis chamber; the second gas flow controller includes: a large flow gas flow controller 292 and a small flow gas flow controller 294, which are used to control the flow rate of the carrier gas into the hydrogen analysis chamber during the hydrogen measurement, or the flow rate of the hydrogen-containing calibration gas into the hydrogen analysis chamber during calibration. According to this embodiment of the present invention, the specific type of the corresponding flow controller is not limited, as long as the flow control function can be realized. It can be understood that the large flow and the small flow of the present invention are relative, and the specific requirements are subject to the actual requirements. For example: when the flow rate of the small flow is 0-200mL / min, the flow rate of the large flow exceeds 200mL / min.

[0076] In this embodiment, the vacuum pump module is a vacuum pump 20 .

[0077] Continue to refer to Figure 7As shown, the gas circuit connection mode of each module of the gas supply device is as follows: the carrier gas source 231, the high hydrogen concentration calibration gas source 232, and the low hydrogen concentration calibration gas source 233 are respectively connected to the inlet ends of the first pressure reducing valve 241, the second pressure reducing valve 242, and the third pressure reducing valve 243, the carrier gas solenoid valve 251, the first hydrogen-containing calibration gas solenoid valve 252, and the second hydrogen-containing calibration gas solenoid valve 253 are respectively connected to the outlet ends of the first pressure reducing valve 241, the second pressure reducing valve 242, and the third pressure reducing valve 243, and the outlet gas circuits of the three solenoid valves are combined and simultaneously connected to the inlet of the water vapor removal unit 271, the first gas source pressure gauge 261, and the second gas source pressure gauge 262. The outlet of the water vapor removal unit 271 is connected to the inlet end of the carbon dioxide removal unit 272, and the outlet gas circuit of the carbon dioxide removal unit 272 is simultaneously connected to the first gas flow controller 281, the large flow gas solenoid valve 291, and the small flow gas solenoid valve 293. The gas outlet of the first gas flow controller 281 is connected to the gas inlet of the first gas solenoid valve 282, and the gas outlet of the first gas solenoid valve 282 is connected to the gas inlet 15 of the sample pre-release area of ​​the hydrogen evolution chamber. The gas outlet of the large-flow gas solenoid valve 291 is connected to the gas inlet of the large-flow gas flow controller 292, and the gas outlet of the large-flow gas flow controller 292 is connected to the gas inlet 11 of the heating zone of the hydrogen evolution chamber. The gas outlet of the small-flow gas solenoid valve 293 is connected to the gas inlet of the small-flow gas flow controller 294, and the gas outlet of the small-flow gas flow controller 294 is connected to the gas inlet 11 of the heating zone of the hydrogen evolution chamber. A hydrogen evolution chamber pressure gauge 30 is provided at the gas inlet 11 of the heating zone of the hydrogen evolution chamber 36 for obtaining the gas pressure in the hydrogen evolution chamber. The heating zone gas outlet 12 of the hydrogen evolution chamber 36 is connected to the gas inlet of the gas outlet solenoid valve 35, and the gas outlet of the gas outlet solenoid valve 35 is connected to the vacuum pump 20.

[0078] Figure 8 FIG. 1 is a control principle block diagram of a control module in the gas supply device of this embodiment of the present invention, as shown in FIG. Figure 8 As shown, when the air supply device in this embodiment is used for the detection device of Example 1, the control module is connected to the control processing system of the detection device of Example 1. It can be understood that the control module and the control processing system can also be combined into a control processing unit for unified control.

[0079] The control module can be a PLC, an industrial control computer, a personal computer or an embedded processor. In this embodiment, an industrial control computer is preferred. Figure 8As shown, the control module includes: a processor 31, a signal conversion module 32, a switch input and output module 33 and an analog input module 34. When the gas supply device is working, each module is controlled by the processor. The processor 31 is connected with the switch input and output module 33, the analog input module 34, the first gas flow controller 281, the large flow gas flow controller 292 and the small flow gas flow controller 294 through the signal conversion module 32 to realize the control of each solenoid valve of the gas solenoid valve module and the vacuum pump 20, and obtain the pressure signal data sent back by the first gas source pressure gauge 261 and the hydrogen evolution chamber pressure gauge 30.

[0080] It is understandable that, in this embodiment of the present invention, the types of the signal conversion module, the switch input and output module, and the analog input module are not particularly limited, as long as they can achieve their corresponding functions.

[0081] Example 4: According to this embodiment of the present invention, there is provided a gas supply method for detecting the hydrogen content in solid metal using the gas supply device described in the aforementioned Example 3, which specifically includes: before starting to detect the hydrogen content in the solid metal, the control module controls the switch input and output module to close the first hydrogen-containing calibration gas solenoid valve 252 and the second hydrogen-containing calibration gas solenoid valve 253, opens the carrier gas solenoid valve 251, adjusts the first pressure reducing valve 241, and observes the second gas source pressure gauge 262 at the same time until the pressure reaches slightly greater than one atmosphere. After the solid metal sample is placed in the sample pre-discharge area 101 of the hydrogen evolution chamber, the first gas solenoid valve 282, the large-flow gas solenoid valve 291 and the small-flow gas solenoid valve 293 are closed, the gas outlet solenoid valve 35 is opened, the first gas flow controller 281 is set to reach a certain gas flow rate, and then the vacuum pump 20 is opened to evacuate the hydrogen evolution chamber to exhaust most of the air from the hydrogen evolution chamber, and then the gas outlet solenoid valve 35 and the vacuum pump 20 are closed to put the hydrogen evolution chamber in a certain vacuum state, and then the first gas solenoid valve 282 is opened again to allow the carrier gas in the carrier gas source 231 to flow into the hydrogen evolution chamber through the first gas solenoid valve 282. During the inflow process, the pressure of the hydrogen evolution chamber pressure gauge 30 gradually increases. When the pressure is greater than one atmospheric pressure, the gas outlet solenoid valve 35 is opened, and the carrier gas is continuously purged and discharged through the hydrogen evolution chamber to achieve purging and removal of impurity gases adsorbed on the surface of the solid metal sample, and the hydrogen evolution chamber is filled with flowing carrier gas. After purging for a certain period of time, the solid metal sample is moved from the sample pre-discharge area 101 of the hydrogen evolution chamber into the heating area 102 of the hydrogen evolution chamber, and the large flow gas solenoid valve 291 or the small flow gas solenoid valve 293 is opened according to the carrier gas flow rate required for the test, and the first gas solenoid valve 282 is closed, and the large flow gas flow controller 292 or the small flow gas flow controller 294 is adjusted to achieve a suitable flow rate of the carrier gas in the hydrogen evolution chamber, and flow at a certain flow rate in the hydrogen evolution chamber. During the hydrogen precipitation process, the carrier gas gradually takes the precipitated hydrogen out of the hydrogen evolution chamber through the gas outlet solenoid valve 35. After all the hydrogen in the metal sample is precipitated, the large flow gas solenoid valve 291 or the small flow gas solenoid valve 293 is closed, and then the first gas solenoid valve 282 is opened to achieve rapid cooling of the interior of the hydrogen evolution chamber by the carrier gas, so as to prepare for the next sample test.

[0082] Embodiment 5: According to this embodiment of the present invention, a gas supply method for calibrating a high-temperature hydrogen sensor using the gas supply device described in the aforementioned embodiment 3 is provided, which specifically includes: before starting to calibrate the hydrogen content detection device, the control module controls the switch input and output module to open the first hydrogen-containing calibration gas solenoid valve 252 or the second hydrogen-containing calibration gas solenoid valve 253, and close the carrier gas solenoid valve 251 (if a high hydrogen concentration calibration gas is required, the first hydrogen-containing calibration gas solenoid valve 252 is opened and the second hydrogen-containing calibration gas solenoid valve 253 is closed; if a low hydrogen concentration calibration gas is required, the second hydrogen-containing calibration gas solenoid valve 253 is opened and the first hydrogen-containing calibration gas solenoid valve 252 is closed). The second pressure reducing valve 242 or the third pressure reducing valve 243 is adjusted accordingly, and the pressure value displayed by the second gas source pressure gauge 262 is observed at the same time, until the pressure value is slightly greater than one atmosphere. The first gas solenoid valve 282, the large-flow gas solenoid valve 291 and the small-flow gas solenoid valve 293 are closed, and the gas outlet solenoid valve 35 is opened. The control module sets the first gas flow controller 281 to reach a certain gas flow rate, and then the vacuum pump 20 is turned on to evacuate the hydrogen evolution chamber to exhaust most of the air from the hydrogen evolution chamber. Then the gas outlet solenoid valve 35 and the vacuum pump 20 are closed to put the hydrogen evolution chamber in a certain vacuum state. Subsequently, the first gas solenoid valve 282 is opened again to allow the hydrogen-containing calibration gas in the high-hydrogen concentration calibration gas source 232 or the low-hydrogen concentration calibration gas source 233 to flow into the hydrogen evolution chamber through the first gas solenoid valve 282. During the inflow process, the pressure of the hydrogen evolution chamber pressure gauge 30 gradually increases. When the pressure is greater than one atmospheric pressure, the gas outlet solenoid valve 35 is opened, and the hydrogen-containing calibration gas is continuously purged and discharged through the hydrogen evolution chamber, and the hydrogen evolution chamber is filled with flowing hydrogen-containing calibration gas. After purging for a certain period of time, the large-flow gas solenoid valve 291 or the small-flow gas solenoid valve 293 is opened according to the gas flow rate of the hydrogen-containing calibration gas required during calibration, and the first gas solenoid valve 282 is closed, and the large-flow gas flow controller 292 or the small-flow gas flow controller 294 is adjusted to make the hydrogen-containing calibration gas reach a suitable flow rate, so that the hydrogen-containing calibration gas flows in the hydrogen evolution chamber at a certain flow rate. When the temperature inside the hydrogen evolution chamber rises to the test temperature of the high-temperature hydrogen sensor 6, the high-temperature hydrogen sensor 6 detects the hydrogen concentration in the hydrogen evolution chamber, and compares the detection result with the actual hydrogen concentration of the hydrogen-containing calibration gas to achieve calibration of the high-temperature hydrogen sensor 6.

[0083] It can be understood that, in this embodiment, by calibrating the high-temperature hydrogen sensor before detecting the hydrogen content in the solid metal, the detection data of the detection device in Example 1 can be improved, thereby realizing the calibration of the hydrogen content data in the solid metal.

[0084] In summary, the present invention adopts a high-temperature hydrogen sensor that can be directly used at high temperature as a hydrogen measuring element, so that the precipitation and detection of hydrogen in solid metal are carried out simultaneously, and there is no need to collect the precipitated hydrogen before detecting the hydrogen content. This design makes the device more portable and simple; a structural form in which a cylinder branch is provided on the cylinder, and a sample pre-discharge area and a heating area are set for the hydrogen evolution chamber. Before heating and hydrogen evolution, the metal sample to be tested is temporarily placed in the sample pre-discharge area and fully purged by the carrier gas, which can greatly reduce the interference of the adsorbed gas on the sample surface on the hydrogen content detection result; the cooling element can quickly cool the hydrogen evolution chamber, speed up the sample analysis time, and improve the test efficiency; by adding a blank test, the influence of the detection device's own factors on the accuracy of metal hydrogen content detection is reduced. The detection accuracy of the data is improved; the gas supply device can provide carrier gas for the detection of hydrogen content in solid metal samples, and can also provide hydrogen-containing calibration gas for the calibration of high-temperature hydrogen sensors in the detection device. The gas supply process matches the test process and has a high degree of automation; high-hydrogen concentration calibration gas or low-hydrogen concentration calibration gas can be provided to meet the calibration requirements of different hydrogen concentrations, realize the calibration of high-temperature hydrogen sensors, avoid the influence of the sensor's own factors on the accuracy of metal hydrogen content detection, and improve the detection accuracy of the data; by selecting a large-flow flow controller and a small-flow flow controller, the requirements of different gas flow rates entering the hydrogen evolution chamber can be met, the accuracy of gas flow control can be improved, and the calibration process and the accuracy of solid-state metal hydrogen content detection can be further improved.

[0085] In the present invention, unless otherwise clearly specified and limited, the terms "connected", "connection" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0086] In the description of the present invention, it should be understood that the terms "first", "second", "third" and the like are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first", "second", "third" may explicitly or implicitly include one or more of the features.

[0087] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine different embodiments or examples described in this specification and the features of different embodiments or examples without contradiction.

[0088] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations on the present invention. A person skilled in the art may change, modify, replace and modify the above embodiments within the scope of the present invention. At the same time, a person skilled in the art may make changes in the specific implementation methods and scope of application based on the ideas of the present application.

Claims

1. A gas supply device for detecting hydrogen content in solid metal, characterized in that: The gas supply device is used to be connected to a hydrogen evolution chamber for hydrogen evolution of solid metal, and the gas supply device comprises: A gas source module, the gas source module comprising a hydrogen-containing calibration gas source and a carrier gas source; A gas solenoid valve module, the gas solenoid valve module comprising: a carrier gas solenoid valve, a hydrogen-containing calibration gas solenoid valve, a first gas solenoid valve, a second gas solenoid valve and a gas outlet solenoid valve, wherein the carrier gas solenoid valve is connected to the carrier gas source, and the hydrogen-containing calibration gas solenoid valve is connected to the hydrogen-containing calibration gas source; A gas purification module, wherein the inlet of the gas purification module is connected to the carrier gas solenoid valve and the hydrogen-containing calibration gas solenoid valve respectively, the outlet of the gas purification module is connected to the inlet of the first gas solenoid valve via a first gas flow controller, the outlet of the first gas solenoid valve is connected to the gas inlet of the sample pre-release area of ​​the hydrogen evolution chamber, and the outlet of the gas purification module is connected to the inlet of the second gas flow controller via the second gas solenoid valve, and the outlet of the second gas flow controller is connected to the gas inlet of the heating area of ​​the hydrogen evolution chamber; A vacuum pumping module, wherein the vacuum pumping module is connected to the gas outlet of the heating zone of the hydrogen evolution chamber via the gas outlet solenoid valve; A control module, the control module is used for the overall operation of the gas supply device; The hydrogen-containing calibration gas source includes: a high hydrogen concentration calibration gas source with a volume fraction of 10% and a low hydrogen concentration calibration gas source with a volume fraction of 0.1%; the carrier gas stored in the carrier gas source includes: nitrogen or inert gas, and the hydrogen-containing calibration gas stored in the hydrogen-containing calibration gas source is a hydrogen-inert gas mixture.

2. The air supply device according to claim 1, characterized in that: Also includes: A pressure reducing valve module, wherein the carrier gas solenoid valve is connected to the carrier gas source via the pressure reducing valve module, and the hydrogen-containing calibration gas solenoid valve is connected to the hydrogen-containing calibration gas source via the pressure reducing valve module.

3. The air supply device according to claim 2, characterized in that: Also includes: A pressure display module, the pressure display module comprises: a gas source pressure gauge and a hydrogen evolution chamber pressure gauge, the gas source pressure gauge is arranged at the inlet of the gas purification module, and the hydrogen evolution chamber pressure gauge is arranged at the gas inlet of the heating zone of the hydrogen evolution chamber.

4. The air supply device according to claim 3, characterized in that: The gas purification module includes: a water vapor removal unit and a carbon dioxide removal unit, the inlet of the water vapor removal unit is connected to the carrier gas solenoid valve and the hydrogen-containing calibration gas solenoid valve, respectively, the inlet of the carbon dioxide removal unit is connected to the outlet of the water vapor removal unit, and the outlet of the carbon dioxide removal unit is connected to the first gas flow controller and the second gas solenoid valve, respectively.

5. The air supply device according to claim 4, characterized in that: A high-temperature hydrogen sensor for detecting the concentration of hydrogen precipitated from solid metal is provided in the heating zone.

6. The air supply device according to claim 1, characterized in that: The control module is a PLC, an industrial control computer or a personal computer.

7. A gas supply method for detecting hydrogen content in solid metal using the gas supply device according to claim 5, characterized in that: The following steps are involved: S1: Close the hydrogen-containing calibration gas solenoid valve through the control module, open the carrier gas solenoid valve, and adjust the pressure reducing valve module to make the pressure reach slightly greater than one atmosphere; S2: placing the solid metal sample in the sample pre-placement area of ​​the hydrogen evolution chamber, closing the first gas solenoid valve and the second gas solenoid valve, opening the gas outlet solenoid valve at the same time, setting the first gas flow controller to a certain gas flow rate, and then controlling the vacuum pumping module to vacuum the hydrogen evolution chamber, closing the gas outlet solenoid valve and the vacuum pumping module to put the hydrogen evolution chamber in a vacuum state; S3: Open the first gas solenoid valve to allow the carrier gas in the carrier gas source to flow into the hydrogen evolution chamber through the first gas solenoid valve. When the pressure in the hydrogen evolution chamber is greater than one atmosphere, open the gas outlet solenoid valve to allow the carrier gas to continuously purge the solid metal sample and the hydrogen evolution chamber and replace the hydrogen evolution chamber with a carrier gas atmosphere. S4: moving the solid metal sample into the heating zone of the hydrogen evolution chamber, opening the second gas solenoid valve, and closing the first gas solenoid valve, adjusting the second gas flow controller to allow the carrier gas to flow in the hydrogen evolution chamber, and in the process of heating the solid metal sample to precipitate hydrogen, the carrier gas gradually carries the precipitated hydrogen out of the hydrogen evolution chamber through the gas outlet solenoid valve; S5: After all the hydrogen in the solid metal sample is precipitated, the second gas solenoid valve is closed, and then the first gas solenoid valve is opened to continuously purge and cool the interior of the hydrogen evolution chamber with the carrier gas.

8. A gas supply method for calibrating a high-temperature hydrogen sensor using the gas supply device according to claim 5, characterized in that: The following steps are involved: S1: Open the hydrogen-containing calibration gas solenoid valve through the control module, close the carrier gas solenoid valve, and adjust the pressure reducing valve module to make the pressure reach slightly greater than one atmosphere; S2: close the first gas solenoid valve and the second gas solenoid valve, open the gas outlet solenoid valve at the same time, set the first gas flow controller to reach a certain gas flow rate, control the vacuum module to vacuum the hydrogen evolution chamber, close the gas outlet solenoid valve and the vacuum module, and put the hydrogen evolution chamber in a vacuum state; S3: Open the first gas solenoid valve to allow the hydrogen-containing calibration gas in the hydrogen-containing calibration gas source to flow into the hydrogen evolution chamber through the first gas solenoid valve. When the pressure in the hydrogen evolution chamber is greater than one atmosphere, open the gas outlet solenoid valve to allow the hydrogen-containing calibration gas to continuously purge the hydrogen evolution chamber and replace the hydrogen evolution chamber with the hydrogen-containing calibration gas atmosphere. S4: Open the second gas solenoid valve and close the first gas solenoid valve, adjust the second gas flow controller to make the hydrogen-containing calibration gas flow in the hydrogen evolution chamber, and when the temperature inside the hydrogen evolution chamber reaches the test temperature of the high-temperature hydrogen sensor, the high-temperature hydrogen sensor detects the hydrogen concentration in the hydrogen evolution chamber, and compares the detection result with the actual hydrogen concentration of the hydrogen-containing calibration gas to achieve calibration of the high-temperature hydrogen sensor.

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