Experimental platform for testing gas behavior of material

Abstract

The utility model relates to the technical field of material test and preparation, in particular to a gas behavior test experimental platform for materials, which comprises a gas supply system, a vacuum pump system, a detection mechanism, a reaction generation mechanism and at least more than two types of reaction generation mechanisms, at least one mounting position matched with the reaction generation mechanism is arranged in the reaction generation mechanism, the reaction generation mechanism is connected with a heating mechanism, the gas supply system, the vacuum pump system and the detection mechanism are respectively communicated with a pipeline of the reaction generation mechanism, a plurality of valves are arranged on the pipeline, and a flow meter and a pressure meter are arranged between the gas supply system and the reaction generation mechanism. The test platform is adopted in the test method. One experiment platform can complete various experiments, test cost and space resources are reduced, material test efficiency is improved, meanwhile, preparation of the metal hydride and desorption test of the prepared metal hydride can be carried out, a sample can be continuously subjected to test experiments after preparation, and the accuracy of a test result is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to material testing and preparation technical field, especially relate to a material's gas behavior test experiment platform. BACKGROUND

[0002] The existing material gas behavior test mainly has thermal desorption method (TDS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) etc., usually all need to be completed under the cooperation of high vacuum background and mass spectrometer, to use the thermal desorption spectrum method (TDS) that gas behavior research test in material is usually taken as an example, this experiment mainly utilizes mass spectrometer to capture the gas signal released under the high vacuum degree background of sample.The device used for the existing material gas behavior test is all single for each kind of test, and the device function of each test is single, when needing to carry out a plurality of types of gas behavior test, different devices need to be prepared for different tests, leading to higher test cost, and the device occupies larger space in laboratory, simultaneously, the material used for carrying out gas behavior test needs to be prepared separately before testing, and then is transferred to the device for testing, needs to be equipped with special preparation equipment, and some more active materials are easy to react with air in the transfer process, and then the final test result of material can be deviated from the actual situation, influence material's test and application. UTILITY MODEL CONTENT

[0003] The utility model is aimed at: the device function of the existing gas behavior test is single, leading to higher test cost, and occupying larger space in laboratory, and the material needs to be transferred in the testing process after preparation, and is easy to contact air and influence test result technical problem, provide a material's gas behavior test experiment platform.

[0004] In order to realize the above-mentioned purpose, the utility model adopts the technical scheme that:

[0005] A material's gas behavior test experiment platform, including gas supply system, vacuum pump system, detection mechanism and at least two kinds of above type reaction generating mechanism, the reaction generating mechanism is connected with heating mechanism, the gas supply system, the vacuum pump system and the detection mechanism are connected with the reaction generating mechanism pipeline respectively, be equipped with a plurality of valves on the pipeline, be equipped with flowmeter and pressure gauge between the gas supply system and the reaction generating mechanism.

[0006] The utility model discloses a material's gas behavior test experiment platform, through the configuration multiple types of reaction generation mechanism, can according to test demand carry out the replacement of reaction generation mechanism, make this experiment platform can satisfy multiple need vacuumizing and heating's gas behavior test experiment, make one experiment platform can complete multiple gas experiments, reduce test cost and space resources, improve the test efficiency of material, simultaneously, through the valve control the intercommunication state of each part, can realize the change of reaction generation mechanism's internal environment, make the preparation of metal hydride in reaction generation mechanism, also can carry out the desorption test of prepared metal hydride, make sample can continuously carry out the follow -up test experiment after preparation without contacting air, improve the accuracy of test result.

[0007] As the preferred scheme of the utility model, the heating mechanism can provide at least the working temperature from room temperature to 1100 DEG C for the reaction generation mechanism. To provide the required test environment.

[0008] As the preferred scheme of the utility model, the vacuum pump system includes molecular pump and pre-pump connected in sequence, and the vacuum pump system can provide at least 10 -5 Pa vacuum degree working environment for the reaction generation mechanism. To provide the required test environment.

[0009] As the preferred scheme of the utility model, the reaction generation mechanism includes double opening quartz tube, double opening flange stainless steel pipe and single opening quartz tube, the double opening quartz tube can be used for sample preparation of metal hydride, the double opening flange stainless steel pipe can be used for sample airtightness test, and the single opening quartz tube can be used for sample TDS experiment. The setting of multiple reaction generation mechanisms provides the required test environment for different materials and different test requirements.

[0010] As the preferred scheme of the utility model, the gas supply system includes hydrogen gas supply mechanism and helium gas supply mechanism, and the hydrogen gas supply mechanism and the helium gas supply mechanism are communicated with the reaction generation mechanism. To improve different types of test gas, realize sample preparation and test under the action of different types of gas.

[0011] As the preferred scheme of the utility model, the gas supply system includes several gas cylinders, the gas cylinder is connected with gas quantitative accumulator, the gas quantitative accumulator is communicated with the reaction generation mechanism, the flowmeter is arranged between the gas cylinder and the gas quantitative accumulator, and the pressure gauge is connected with the gas quantitative accumulator. Through the combination of gas cylinder and quantitative accumulator, the test platform can be provided with sufficient test gas through the gas cylinder, and the test platform can be provided with a set amount of test gas through the quantitative accumulator, so as to meet sample preparation and test under different conditions.

[0012] Therefore, the material gas behavior test experiment platform has the advantages that:

[0013] 1、 The material gas behavior test experiment platform of the utility model, through configuration multiple types of reaction occurrence mechanism, can change reaction occurrence mechanism in reaction occurrence mechanism according to test demand, make this experiment platform can satisfy multiple need vacuumizing and heating's gas behavior test experiment, make one experiment platform can complete multiple gas experiments, reduce test cost and space resource, improve material's test efficiency;

[0014] 2、 The material gas behavior test experiment platform of the utility model, through valve control each part's intercommunication state, can realize reaction occurrence mechanism in the change of environment, make reaction occurrence mechanism in can prepare metal hydride, also can prepare the desorption test of metal hydride, make sample can continuously carry out subsequent test experiment after preparation without contacting air, improve the accuracy of test result. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a kind of material's gas behavior test experiment platform's structural schematic diagram of the utility model;

[0016] Figure: 1-gas supply system, 11-hydrogen gas supply mechanism, 12-helium gas supply mechanism, 13-gas quantitative storage, 2-vacuum pump system, 21-molecular pump, 22-prepump, 3-detection mechanism, 4-reaction occurrence mechanism, 41-double opening quartz tube, 42-double opening flange stainless steel tube, 43-single opening quartz tube, 5-heating mechanism, 6-valve, 7-flow meter, 8-pressure gauge, 9-vacuum gauge. DETAILED DESCRIPTION

[0017] The utility model will be specifically explained in combination with the drawings.

[0018] In order to make the purpose, technical scheme and advantage of the utility model more clearly, the following is in combination with the drawings and example, and the utility model is further specifically explained.It should be understood that the specific embodiments described herein are only used to explain the utility model, and are not used to limit the utility model.

[0019] Example 1

[0020] As Figure 1As shown, a material gas behavior test experiment platform includes a gas supply system 1, a vacuum pump system 2, a detection mechanism 3 and at least two reaction occurrence mechanisms 4, the reaction occurrence mechanism 4 is connected with a heating mechanism 5, the gas supply system 1, the vacuum pump system 2 and the detection mechanism 3 are respectively communicated with the reaction occurrence mechanism 4 through pipelines, and a plurality of valves 6 are arranged on the pipelines, and the gas supply system 1 is provided with a flow meter 7 and a pressure gauge 8 between the gas supply system 1 and the reaction occurrence mechanism 4.

[0021] The gas supply system 1 is used to provide a gas source for the experiment platform, and the gas supply system 1 can be a combination of a plurality of gas cylinders connected with the reaction occurrence mechanism 4 through pipelines.

[0022] Preferably, the pipeline between the gas cylinder of the gas supply system 1 and the reaction occurrence mechanism 4 is provided with a valve 6, so that different gas cylinders can be used for gas supply according to actual conditions, and different types of gas can be filled in different gas cylinders according to actual conditions to meet different experimental requirements.

[0023] Preferably, the pipeline between the gas cylinder of the gas supply system 1 and the reaction occurrence mechanism 4 is provided with a flow meter 7, so that the flow rate of the gas flow output by the gas cylinder can be adjusted according to actual conditions to realize the reaction occurrence mechanism 4 to improve the constant speed of the gas flow to meet the experimental requirements of specific requirements.

[0024] Preferably, the gas supply system 1 can include a hydrogen gas supply mechanism 11 and a helium gas supply mechanism 12, and the hydrogen gas supply mechanism 11 and the helium gas supply mechanism 12 can be two independently arranged gas cylinders respectively communicated with the reaction occurrence mechanism 4 through pipelines with valves 6 to provide different types of test gases to realize sample preparation and testing under the action of different types of gases.

[0025] Preferably, the gas supply system 1 can further include a gas quantitative storage device 13, the gas quantitative storage device 13 is a container with a known volume, the gas quantitative storage device 13 can be communicated with the pipeline of the gas cylinder, the gas can be filled into the gas quantitative storage device 13 through the gas cylinder, and the gas can be temporarily stored in the gas quantitative storage device 13, and the pressure gauge 8 can be connected to the gas quantitative storage device 13, and the pressure of the gas in the gas quantitative storage device 13 can be read through the pressure gauge 8 to calculate the amount of the gas stored therein, so as to provide a constant amount of gas for the reaction occurrence mechanism 4 to meet the sample preparation and testing under the action of different amounts of gas.

[0026] Preferably, the flow meter 7 can be arranged between the gas cylinder and the gas quantitative storage device 13, the pressure gauge 8 can be connected to the gas quantitative storage device 13, and the pressure gauge 8 can also be arranged between the gas quantitative storage device 13 and the reaction occurrence mechanism 4. Through the combination of the gas cylinder and the quantitative storage device, the test platform can be provided with sufficient test gas through the gas cylinder, and the test platform can also be provided with a set amount of test gas through the quantitative storage device to meet the sample preparation and testing under different conditions.

[0027] The heating mechanism 5 is used to heat the reaction occurrence mechanism 4 to a specified working temperature.

[0028] Preferably, the heating mechanism 5 can at least provide the reaction occurrence mechanism 4 with a working temperature in the range from room temperature to 1100℃. To provide a test environment that meets the requirements.

[0029] Preferably, the heating mechanism 5 can be a tube furnace, in particular a multi-temperature-zone tube furnace, which can be set to different temperatures according to different process requirements, and is provided with multiple temperature display and control instruments on the furnace body to realize temperature adjustment and display. The reaction occurrence mechanism 4 is clamped in the tube furnace and can maintain a stable working temperature under the action of the tube furnace.

[0030] The vacuum pump system 2 is used to perform vacuum pumping operation on the experimental platform to meet the required vacuum degree of the experiment.

[0031] Preferably, the vacuum pump system 2 can include a molecular pump 21 and a backing pump 22 connected in sequence, and a vacuum gauge 9 is arranged on the pipeline in a matched manner. The vacuum pump system 2 can at least provide the reaction occurrence mechanism 4 with a working environment of 10-5Pa vacuum degree.

[0032] The reaction occurrence mechanism 4 is a carrier mechanism for containing test materials, which is a container structure for the reaction and test of materials under a set temperature and vacuum degree. Different experiments can be met by replacing the reaction occurrence mechanism 4 in the middle of the experimental platform.

[0033] Preferably, the reaction occurrence mechanism 4 can include a double-opening quartz tube 41, a double-opening flange stainless steel tube 42, and a single-opening quartz tube 43. The double-opening quartz tube 41 can be used for sample preparation of metal hydride. The double-opening flange stainless steel tube 42 can be used for air tightness test of the sample. The single-opening quartz tube 43 can be used for TDS experiment of the sample. The simultaneous arrangement of multiple reaction occurrence mechanisms 4 can provide a test environment that meets the requirements of different materials and different test requirements.

[0034] Preferably, when the double-opening quartz tube 41 is used, the required product can be generated by gas reacting with the base material in an environment of high vacuum degree and required working temperature, for example, metal hydride can be prepared in this environment.

[0035] Specifically, taking the preparation of metal hydride by using double-open quartz tube 41 as an example, first, the entire system of the experimental platform is pumped to the required vacuum degree by the vacuum pump system 2, then the quartz tube is heated to the specified temperature by the tube furnace, hydrogen gas stored in the gas quantitative storage mechanism in advance is introduced, the hydrogen gas reacts with the metal in the quartz tube, and the pressure change from before the reaction to the end of the reaction is recorded by the pressure gauge 8, so that the amount of hydrogen absorbed by the sample can be calculated, thereby realizing the preparation of the sample under quantitative hydrogen charging.

[0036] Specifically, taking the preparation of large-size and high-concentration metal hydride by using double-open quartz tube 41 as an example, the large-size and high-concentration material sample can be a large cylinder with a diameter of 30 mm and a length of 50 mm. At this time, if the quantitative hydrogen charging method is continued, a large pressure of hydrogen gas is required, and the direct contact of the hydrogen gas with the sample at too high a pressure will cause the sample to crack, which cannot guarantee the quality of the prepared metal hydride and affects the smooth progress of the preparation process. Therefore, the flow rate of the charged hydrogen gas is controlled by the flow meter 7 to avoid the cracking of the sample due to the too fast charging of the hydrogen gas, thereby realizing the preparation of the sample under constant-speed hydrogen charging.

[0037] Preferably, when the double-open flange stainless steel tube 42 is used, the sample can be packaged on the carrier by the two stainless steel tube clamping carriers, and the high-vacuum airtightness measurement can be performed.

[0038] Specifically, taking the tubular sample as an example, the tubular sample can be connected to the two double-open flange stainless steel tubes 42 through the sealed assembly of the sample and the carrier and the connection with the flange. The two double-open flange stainless steel tubes 42 are connected to the left and right ends of the sample carrier respectively, the left stainless steel tube is connected to the gas supply system 1, and the right stainless steel tube is connected to the detection mechanism 3. The tubular wall of the tubular sample is used as a barrier to divide the vacuum pump system 2 into left and right space parts. The appropriate amount of helium gas, for example, 10 Pa-1.5×106 Pa, is charged into the left part, and at the same time, it is observed whether the mass spectrometer on the right detects the rising helium signal, so as to realize the airtightness test of the sample. If other types of samples, such as cylinders, discs, etc., need to be detected, the intermediate reaction occurrence mechanism 4 and the sealing method can be replaced so that the sample can be connected to the double-open flange stainless steel tube 42 and the vacuum system is divided, and then the airtightness detection is performed.

[0039] Preferably, when the single-open quartz tube 43 is used, the entire system of the experimental platform can reach the range in which the mass spectrometer can normally work by the vacuum pump system 2. The quartz tube is heated by the tube furnace, and the sample will release gas. The released gas signal will be detected by the mass spectrometer, and then the TDS experiment is smoothly performed.

[0040] The detection mechanism 3 is a gas signal detection mechanism 3 matched with the experimental platform, which is used for detecting the gas signal in the reaction or test process.

[0041] Preferably, the detection mechanism 3 can be a quadrupole mass spectrometer.

[0042] Preferably, the mass spectrometer can determine whether the sample leaks according to whether the inflation gas signal is detected during the airtightness test of the sample, and can also perform thermal desorption analysis by capturing the gas signal released by the sample in a high vacuum background.

[0043] The gas behavior test experiment platform of one material of the embodiment can be divided into left, middle and right three parts according to functions as a whole. The left part is the gas supply system 1, the middle part is the reaction occurrence mechanism 4, and the right part is the vacuum pump system 2 and the detection mechanism 3. The parts are connected through metal pipes. Valves 6 are arranged on the pipes between the components, so that the components can be connected or cut off according to the actual situation, can be opened and closed according to the experimental process, and can be isolated in time in case of unexpected situations to ensure the safety of the experimental platform. When in use, the vacuum pump system 2 maintains the vacuum environment in the reaction occurrence mechanism 4, the gas supply system 1 supplies gas source for the middle reaction occurrence mechanism 4, the material reacts or tests in the reaction occurrence mechanism 4, the detection mechanism 3 detects according to the actual situation, and the reaction occurrence mechanism 4 is replaced according to the actual detection requirement.

[0044] The gas behavior test experiment platform of one material of the embodiment can be divided into left, middle and right three parts according to functions as a whole. The left part is the gas supply system 1, the middle part is the reaction occurrence mechanism 4, and the right part is the vacuum pump system 2 and the detection mechanism 3. The parts are connected through metal pipes. Valves 6 are arranged on the pipes between the components, so that the components can be connected or cut off according to the actual situation, can be opened and closed according to the experimental process, and can be isolated in time in case of unexpected situations to ensure the safety of the experimental platform. When in use, the vacuum pump system 2 maintains the vacuum environment in the reaction occurrence mechanism 4, the gas supply system 1 supplies gas source for the middle reaction occurrence mechanism 4, the material reacts or tests in the reaction occurrence mechanism 4, the detection mechanism 3 detects according to the actual situation, and the reaction occurrence mechanism 4 is replaced according to the actual detection requirement.

[0045] Embodiment 2

[0046] A gas behavior test experiment method of one material, which adopts the gas behavior test experiment platform of one material of embodiment 1 and comprises the following steps:

[0047] S1, preparing the reaction occurrence mechanism 4 according to the test requirement, and setting the sample to be tested in the reaction occurrence mechanism 4;

[0048] S2, providing a working environment meeting the vacuum degree requirement for the reaction occurrence mechanism 4 by the vacuum pump system 2;

[0049] S3, heating the reaction generating mechanism 4 to a specified temperature by the heating mechanism 5;

[0050] S4, sample preparation of metal hydride, gas tightness test or TDS experiment according to test requirements; sample preparation, gas tightness test and TDS experiment are respectively carried out by replacing the reaction generating mechanism 4, or sample preparation and TDS experiment are continuously carried out without replacing the reaction generating mechanism 4.

[0051] Preferably, the sample preparation of metal hydride includes: setting the metal to be reacted in the reaction generating mechanism 4, storing a certain amount of hydrogen in the gas quantitative storage 13, connecting the reaction generating mechanism 4 and the double-opening quartz tube 41, recording the pressure change in the reaction generating mechanism 4 before and after the reaction of the sample to be tested and hydrogen by the pressure gauge 8, calculating the amount of hydrogen absorbed by the sample to be tested, and realizing the reaction of hydrogen filled quantitatively.

[0052] Preferably, the sample preparation of metal oxide includes: setting the metal to be reacted in the reaction generating mechanism 4, connecting the reaction generating mechanism 4 and the double-opening quartz tube 41, and realizing the reaction of hydrogen filled at a constant speed by the flow meter 7. The metal hydride preparation under the constant speed of hydrogen filling can avoid the cracking of the sample caused by the excessive pressure of hydrogen filled, and can meet the preparation of metal hydride with larger size and purity.

[0053] Preferably, the TDS experiment includes disconnecting the connection between the gas supply system 1 and the reaction generating mechanism 4, heating the reaction generating mechanism 4 to the working temperature by the heating mechanism 5 in the working environment with the required vacuum degree, and detecting the overflow gas signal by the detection mechanism 3; the gas tightness test includes filling helium into one side of the reaction generating mechanism 4 by the gas supply system 1, and detecting the helium signal by the detection mechanism 3 on the other side.

[0054] The material gas behavior test experiment method of the embodiment can meet different types of gas behavior tests of different materials by using the experimental platform, can improve the efficiency and accuracy of the experimental process by the functional coupling of the experimental platform, can continuously carry out the detection after the sample preparation, and can improve the accuracy of the experimental results.

[0055] The above only describes the preferred embodiments of the utility model, and does not limit the utility model, and any modification, equivalent replacement and improvement made within the spirit and principle of the utility model should be included in the protection scope of the utility model.

Claims

1. A test platform for gas behavior of a material, characterized in that, The system comprises a gas supply system (1), a vacuum pump system (2), a detection mechanism (3), and at least two reaction generating mechanisms (4), the reaction generating mechanism (4) is connected with a heating mechanism (5), the gas supply system (1), the vacuum pump system (2) and the detection mechanism (3) are respectively communicated with the reaction generating mechanism (4) through pipelines, a plurality of valves (6) are arranged on the pipelines, a flow meter (7) and a pressure gauge (8) are arranged between the gas supply system (1) and the reaction generating mechanism (4).

2. The test platform for gas behavior of a material of claim 1, wherein, The heating mechanism (5) can at least provide the reaction generating mechanism (4) with a working temperature ranging from room temperature to 1100℃.

3. A test platform for gas behavior of a material as claimed in claim 2, wherein, The vacuum pump system (2) comprises a molecular pump (21) and a backing pump (22) connected in sequence, and the vacuum pump system (2) can at least provide the reaction generating mechanism (4) with a working environment of 10-5Pa vacuum degree.

4. The test platform for gas behavior of a material of claim 3, wherein, The reaction generating mechanism (4) comprises a double-opening quartz tube (41), a double-opening flange stainless steel tube (42) and a single-opening quartz tube (43), the double-opening quartz tube (41) can be used for sample preparation of metal hydride, the double-opening flange stainless steel tube (42) can be used for airtightness test of the sample, and the single-opening quartz tube (43) can be used for TDS experiment of the sample.

5. A test rig for gas behaviour of a material as claimed in any of claims 1 to 4, characterised in that, The gas supply system (1) comprises a hydrogen gas supply mechanism (11) and a helium gas supply mechanism (12), and the hydrogen gas supply mechanism (11) and the helium gas supply mechanism (12) are respectively communicated with the reaction generating mechanism (4).

6. A test platform for gas behavior of a material as claimed in claim 5, wherein, The gas supply system (1) comprises a plurality of gas cylinders, the gas cylinders are connected with a gas quantitative storage device (13), the gas quantitative storage device (13) is communicated with the reaction generating mechanism (4), the flow meter (7) is arranged between the gas cylinders and the gas quantitative storage device (13), and the pressure gauge (8) is connected with the gas quantitative storage device (13).

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