CN113466427A - Experimental system for testing hydrogen brittleness resistance and service life of material in high-pressure hydrogen environment - Google Patents

Experimental system for testing hydrogen brittleness resistance and service life of material in high-pressure hydrogen environment Download PDF

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CN113466427A
CN113466427A CN202110768665.7A CN202110768665A CN113466427A CN 113466427 A CN113466427 A CN 113466427A CN 202110768665 A CN202110768665 A CN 202110768665A CN 113466427 A CN113466427 A CN 113466427A
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hydrogen
gas
kettle
pressure gas
cylinder
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邢潇
苟金鑫
崔淦
刘建国
李自力
聂如煜
邓翔元
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China University of Petroleum East China
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China University of Petroleum East China
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Abstract

The invention provides a hydrogen embrittlement resistance test experiment system for a material, which belongs to the technical field of material performance test and comprises a slow strain rate tensile testing machine; the high-pressure gas kettle is arranged on the slow strain rate tensile testing machine and is connected with a hydrogen cylinder, a nitrogen cylinder and a third type gas cylinder through a gas loop control system; injecting the gases in the hydrogen cylinder, the nitrogen cylinder and the third type gas cylinder into the high-pressure gas kettle at different partial pressures through a gas loop control system; a constant temperature circulator for controlling the temperature of the high pressure gas kettle; an oxygen concentration detector for detecting the oxygen concentration in the high-pressure gas kettle; and the combustor is used for combusting the hydrogen-containing waste gas discharged by the high-pressure gas kettle. The device can realize the hydrogen embrittlement slow strain rate stretching and low cycle cyclic load fatigue experiment of the material under the environment of multi-component high-pressure gas, has a large temperature and pressure control range, has a waste gas treatment system, can alarm and treat the leakage condition of combustible gas, and has good safety.

Description

Experimental system for testing hydrogen brittleness resistance and service life of material in high-pressure hydrogen environment
Technical Field
The invention relates to the technical field of material performance testing, in particular to a hydrogen embrittlement resistance and service life testing experimental system for a material in a high-pressure hydrogen environment.
Background
In the service process of the metal pipeline, hydrogen is separated out through cathodic protection or hydrogen is conveyed in a future high-pressure natural gas pipeline in a hydrogen-doped mode, so that hydrogen atoms can permeate into metal, and the hydrogen enters the metal and then interacts with a metal matrix to cause the reduction of mechanical properties such as toughness and plasticity, so that the material is brittle or cracked, namely the hydrogen embrittlement phenomenon of the material. The method for testing the mechanical property of the material after being charged with hydrogen is an important means for researching the hydrogen brittleness problem. In view of the danger of hydrogen and the high possibility of explosion after mixing with oxygen, reasonable measures should be adopted to control the high-pressure hydrogen charging and the material mechanical property testing process so as to improve the safety and reliability of the experiment.
The existing device for testing the mechanical property of the material under the high-pressure hydrogen charging environment can only perform material fracture toughness or fatigue test, the temperature and pressure control range is small, in addition, the existing device does not consider dangers caused by leakage of hydrogen and other combustible gases in a laboratory, and has no waste gas treatment system, and the device is large in limitation.
Disclosure of Invention
The invention aims to provide a test system for hydrogen embrittlement resistance and service life of a material under a high-pressure hydrogen environment, which can realize a slow strain rate stretching and low cycle load fatigue test of hydrogen embrittlement of the material under a multi-component high-pressure gas environment, has a large temperature and pressure control range, has a waste gas treatment system, can alarm and treat the leakage condition of combustible gas, and has good safety, so as to solve at least one technical problem in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a system for testing hydrogen brittleness resistance and service life of a material in a high-pressure hydrogen environment, which comprises:
a slow strain rate tensile tester;
a high-pressure gas kettle arranged on the slow strain rate tensile testing machine; the high-pressure gas kettle is connected with a hydrogen cylinder, a nitrogen cylinder and a third type gas cylinder through a gas loop control system; injecting the gases in the hydrogen cylinder, the nitrogen cylinder and the third type gas cylinder into the high-pressure gas kettle at different partial pressures through the gas loop control system;
a constant temperature circulator for controlling the temperature of the high pressure gas kettle;
an oxygen concentration detector for detecting the oxygen concentration in the high-pressure gas kettle;
and the combustor is used for combusting the hydrogen-containing waste gas discharged by the high-pressure gas kettle.
Preferably, the high-pressure gas kettle comprises an inner kettle body and an outer temperature control medium jacket, and the constant-temperature circulator is connected with the outer temperature control medium jacket of the high-pressure gas kettle through a pipeline.
Preferably, the material of the inner layer kettle body is hastelloy C276.
Preferably, the gas loop control system comprises a compressor, gas path switching valves are arranged on pipelines between the compressor and the hydrogen cylinder, between the compressor and the third type of gas cylinder, and the compressor is connected with an exhaust valve.
Preferably, the slow strain rate tensile testing machine, the high-pressure gas kettle, the gas loop control system, the constant-temperature circulator, the hydrogen cylinder, the nitrogen cylinder and the third type gas cylinder are arranged in a laboratory.
Preferably, the top of laboratory is equipped with explosion-proof formula frequency conversion air exhauster, explosion-proof formula frequency conversion air exhauster's control system is connected with baroceptor, baroceptor is used for detecting the inside atmospheric pressure of laboratory.
Preferably, the control system of the explosion-proof variable-frequency exhauster is further connected with a hydrogen concentration detector, and the hydrogen concentration detector is used for detecting the concentration of hydrogen in the laboratory.
Preferably, when the hydrogen detector detects that the concentration of hydrogen in the laboratory reaches a preset threshold value, the control system controls the experiment power supply to be cut off, and meanwhile, the exhaust volume of the explosion-proof variable-frequency exhauster is increased.
Preferably, the control system of the explosion-proof variable-frequency exhauster is further connected with an alarm, and when the hydrogen detector detects that the concentration of hydrogen in the laboratory reaches a preset threshold value, the control system controls the alarm to give an alarm.
Preferably, when the oxygen concentration detector detects that the oxygen concentration in the high-pressure gas kettle exceeds a preset threshold, the cyclic operation of 'nitrogen purging, nitrogen pressurizing, evacuation and exhaust, and nitrogen purging' of the high-pressure gas kettle is realized through the process switching of the gas loop control system, so that the oxygen concentration in the high-pressure gas kettle is reduced.
The invention has the beneficial effects that:
the device can be used for performing the slow stretching and low cycle fatigue test of the hydrogen embrittlement of the material in a multi-component high-pressure gas environment, and can control the test temperature and pressure conditions;
through the waste gas treatment system, the combustible gas burner carries out combustion treatment on the hydrogen-containing waste gas, and water generated by combustion can be discharged harmlessly;
the laboratory environment is maintained in a micro-negative pressure state through the explosion-proof negative pressure variable frequency exhaust system, and the combustible gas can be exhausted outdoors in time due to trace leakage, so that the danger caused by the leakage of the combustible gas is reduced;
through combustible gas leakage warning and safety control system, when combustible gas leaks, guarantee personnel and laboratory safety through audible and visual warning, cut off experiment power and increase explosion-proof formula frequency conversion air exhauster displacement, further improved the security of experiment.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a structural diagram of a hydrogen embrittlement resistance and life test experiment system of a material in a high-pressure hydrogen environment according to an embodiment of the present invention.
FIG. 2 is a block diagram of a high pressure gas autoclave in accordance with an embodiment of the present invention.
Wherein: 1-an air pressure sensor; 2-explosion-proof variable frequency exhauster; 3-hydrogen concentration detector; 4-an alarm; 5-hydrogen gas cylinder; 6-nitrogen gas cylinder; 7-a third type gas cylinder; 8-gas loop control system; 9-slow strain rate tensile tester; 10-oxygen concentration detector; 11-high pressure gas kettle; 12-a constant temperature circulator; 13-a burner; 14-a housing; 15-inner container; 16-an inlet; 17-an outlet; 18-valve g interface; 19-valve h interface; 20-valve i interface; 21-oxygen concentration detector interface.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below by way of the drawings are illustrative only and are not to be construed as limiting the invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
In the description of the present specification, the terms "first", "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description of the present specification, the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, only for convenience of description and simplification of description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present technology.
Unless expressly stated or limited otherwise, the terms "mounted," "connected," "coupled," and "disposed" are intended to be inclusive and mean, for example, that they may be fixedly coupled or disposed, or that they may be removably coupled or disposed, or that they may be integrally coupled or disposed. The specific meaning of the above terms in the present technology can be understood by those of ordinary skill in the art as appropriate.
For the purpose of facilitating an understanding of the present invention, the present invention will be further explained by way of specific embodiments with reference to the accompanying drawings, which are not intended to limit the present invention.
It should be understood by those skilled in the art that the drawings are merely schematic representations of embodiments and that the elements shown in the drawings are not necessarily required to practice the invention.
Example 1
In this embodiment 1, a system for testing hydrogen embrittlement in a material under an environment of high-pressure hydrogen and other mixed gases and low cycle fatigue is provided, which includes: the device comprises a gas cylinder, a gas loop control system, a slow strain rate tensile testing machine, a high-pressure gas kettle, an oxygen concentration detector, a high-low temperature constant-temperature circulator, a combustible gas burner, an explosion-proof negative pressure variable-frequency exhaust system and a combustible gas leakage alarm and safety control system.
The gas cylinders comprise a nitrogen cylinder, a hydrogen cylinder and a third type gas cylinder.
The gas loop control system is connected with the gas cylinder and the high-pressure gas kettle through pipelines, and the gas in the gas cylinder and the gas loop control system can be used for pressurizing or vacuumizing the high-pressure gas kettle.
The slow strain rate tensile testing machine can be used for carrying out slow strain tensile and low cycle cyclic load fatigue tests on metal materials.
The high-pressure gas kettle is arranged on the slow strain rate tensile testing machine, a pressure gauge and a thermometer are arranged on the high-pressure gas kettle, the kettle body comprises an inner kettle body and an outer temperature control medium jacket, the inner kettle body is made of Hastelloy C276, and high-pressure hydrogen and other gas testing environments at set temperature can be realized.
The oxygen concentration detector is installed on the high-pressure gas kettle and used for detecting the oxygen concentration in the high-pressure gas kettle, when the oxygen concentration is too high, the gas loop control system is utilized to carry out nitrogen purging and vacuumizing, the oxygen concentration in the high-pressure gas kettle is ensured within a safety range, and explosion danger caused by mixing of hydrogen and oxygen is prevented.
The high-low temperature constant temperature circulator is connected with the outer temperature control medium jacket of the high-pressure gas kettle through a pipeline and is used for controlling the temperature of the high-pressure gas kettle, the temperature control range is-40-200 ℃, and hydrogen embrittlement experiments under extremely cold conditions and creep experiments under a high-temperature hydrogen embrittlement environment can be realized.
The combustible gas burner is connected with the high-pressure gas kettle through a pipeline, hydrogen-containing waste gas discharged from the high-pressure gas kettle is combusted through the combustible gas burner, and water generated by combustion is discharged from a water pipe at the lower part of the combustible gas burner.
The explosion-proof negative pressure frequency conversion exhaust system comprises a pressure sensor and an explosion-proof frequency conversion exhaust machine, wherein the explosion-proof frequency conversion exhaust machine is provided with a control system, and can exhaust according to the pressure measured by the pressure sensor so as to maintain the indoor state of micro negative pressure, and can ensure that the combustible gas is timely exhausted outdoors when trace leakage occurs.
Combustible gas leakage warning and safety control system include explosion-proof formula negative pressure frequency conversion exhaust system, hydrogen detector and siren, control system set up in the explosion-proof formula frequency conversion exhaust machine, when hydrogen detector detected that indoor hydrogen concentration reaches certain extreme value, control system control experiment power cuts off, through the siren carries out audible and visual alarm, increases simultaneously explosion-proof formula frequency conversion exhaust machine displacement.
In this embodiment 1, the slow strain rate tensile testing machine can perform a constant load creep/stress corrosion test in addition to a slow strain tensile and low cycle load fatigue test of a metal material.
The system described in this embodiment 1 can perform slow stretching and low cycle fatigue tests of hydrogen embrittlement of a material in a multi-component high-pressure gas environment, and can control the test temperature and pressure conditions; through the waste gas treatment system, the combustible gas burner carries out combustion treatment on the hydrogen-containing waste gas, and water generated by combustion can be discharged harmlessly; the laboratory environment is maintained in a micro-negative pressure state through the explosion-proof negative pressure variable frequency exhaust system, and the combustible gas can be exhausted outdoors in time due to trace leakage, so that the danger caused by the leakage of the combustible gas is reduced; through combustible gas leakage warning and safety control system, when combustible gas leaks, guarantee personnel and laboratory safety through audible and visual warning, cut off experiment power and increase explosion-proof formula frequency conversion air exhauster displacement, further improved the security of experiment.
Example 2
As shown in fig. 1, embodiment 2 of the present invention provides a material hydrogen embrittlement resistance test experiment system, which is capable of performing a slow strain rate tensile and low cycle load fatigue test of material hydrogen embrittlement in a multi-component high-pressure gas environment, has a large temperature and pressure control range, has an exhaust gas treatment system, can alarm and handle a combustible gas leakage condition, and has good safety.
The test system for hydrogen embrittlement resistance of the material (a slow stretching and low cycle fatigue test system for hydrogen embrittlement of the material under the environment of high-pressure hydrogen and other mixed gases) comprises:
a slow strain rate tensile tester 9;
a high-pressure gas kettle 11 arranged on the slow strain rate tensile testing machine 9; a hydrogen cylinder 5, a nitrogen cylinder 6 and a third type gas cylinder 7; a gas loop control system 8 connected with the hydrogen cylinder 5, the nitrogen cylinder 6, the third type gas cylinder 7 and the high-pressure gas kettle 11;
a high-low temperature constant temperature circulator 12 connected to the high-pressure gas kettle 11 for controlling the temperature of the high-pressure gas kettle 11;
an oxygen concentration detector 10 disposed on the high-pressure gas kettle 11;
a combustible gas burner 13 connected to the high-pressure gas tank 11;
the explosion-proof type variable frequency exhauster 2 is arranged at the top of the laboratory;
the device comprises an air pressure sensor 1, a hydrogen concentration detector 3 and an alarm 4, wherein the air pressure sensor 1 is arranged at the top of a laboratory and is connected with an explosion-proof variable-frequency exhauster 2.
In this embodiment 2, the gas loop control system 8 can inject the gases in the hydrogen cylinder 5, the nitrogen cylinder 6, and the third type gas cylinder 7 into the high-pressure gas kettle 11 at different partial pressures, and the slow strain rate tensile testing machine 9 can perform slow strain tensile and low cycle cyclic load fatigue tests on the test specimen in a multicomponent high-pressure gas environment.
The high-pressure gas kettle 11 comprises an inner kettle body and an outer temperature control medium jacket, and the high-low temperature constant temperature circulator 12 is connected with the outer temperature control medium jacket of the high-pressure gas kettle 11 through a pipeline and used for controlling the temperature of the high-pressure gas kettle 11, wherein the temperature control range is-40 ℃ to 200 ℃.
The inner kettle body is made of hastelloy C276, has excellent hydrogen embrittlement resistance, and can realize high-pressure hydrogen and other gas test environments at set temperature.
The gas loop control system 8 comprises a compressor, a gas path switching valve and an exhaust valve with noise reduction, and not only can pressurize gas in a gas cylinder and inject the gas into the high-pressure gas kettle 11, but also can realize the vacuum pumping operation of the high-pressure gas kettle 11 through switching processes.
The oxygen concentration detector 10 is installed on the high-pressure gas kettle 11 and can monitor the oxygen concentration in the high-pressure gas kettle 11 in real time, when the oxygen content is high, the cyclic operation of 'nitrogen purging-nitrogen pressurizing-evacuating exhaust-nitrogen purging' can be realized through the flow switching of the gas loop control system 8, the oxygen concentration in the high-pressure gas kettle 11 is reduced, and the safety of an experimental system is ensured.
The pressure sensor 1 reaches the explosion-proof type frequency conversion exhauster 2 constitutes explosion-proof type negative pressure frequency conversion exhaust system, explosion-proof type frequency conversion exhauster 2 is equipped with control system, can exhaust according to the atmospheric pressure that the pressure sensor 1 surveyed to maintain indoor being in little negative pressure state, can guarantee in time to arrange outdoors when taking place combustible gas trace and leak.
Atmospheric pressure sensor 1 explosion-proof formula frequency conversion air exhauster 2 hydrogen detector 3 reaches alarm 4 constitutes combustible gas leakage warning and safety control system, control system set up in explosion-proof formula frequency conversion air exhauster 2, when hydrogen detector 3 detected indoor hydrogen concentration and reached certain extreme value, control system control experiment power cuts off, through alarm 4 carries out acousto-optic warning, increases simultaneously explosion-proof formula frequency conversion air exhauster 2's displacement.
In the embodiment 2, the threshold value is set when the hydrogen concentration in the chamber reaches a certain limit value, and the threshold value can be set according to specific situations.
The combustible gas burner 13 can perform innocent treatment on the mixed hydrogen-containing waste gas after the experiment is finished through combustion, and water generated by combustion can be discharged through a lower water pipe.
The hydrogen embrittlement resistance test experiment system in this embodiment 2 can carry out the slow tensile and low cycle fatigue experiment of material hydrogen embrittlement under the multicomponent high-pressure gas environment, and can control experiment temperature, pressure, is equipped with waste gas innocent treatment system, is equipped with combustible gas in addition and leaks alarm and processing system, and the security is high, and the reliability is strong.
Example 3
As shown in fig. 1, in this embodiment 3, an experimental system for testing hydrogen embrittlement resistance and life of a material in a high-pressure hydrogen environment is provided, the system includes:
a slow strain rate tensile tester 9;
in this example 3, the model of the slow strain rate tensile tester 9 used was WDML-50.
In specific applications, the use model of the slow strain rate tensile testing machine 9 is not limited by the above model, and a technician can select a proper model to use according to specific conditions.
A high-pressure gas kettle 11 arranged on the slow strain rate tensile testing machine 9; the high-pressure gas kettle 11 is connected with a hydrogen cylinder 5, a nitrogen cylinder 6 and a third gas cylinder 7 through a gas loop control system 8; the gases in the hydrogen cylinder 5, the nitrogen cylinder 6 and the third type gas cylinder 7 are injected into the high-pressure gas kettle 11 at different partial pressures through the gas loop control system 8.
A constant temperature circulator 12 for controlling the temperature of the high pressure gas tank 11;
an oxygen concentration detector 10 for detecting the oxygen concentration inside the high-pressure gas kettle 11;
a burner 13 for burning the hydrogen-containing off-gas discharged from the high-pressure gas tank 11.
As shown in fig. 2, in the present embodiment, the structure of the high-pressure gas tank 11 includes: the constant temperature device comprises a shell 14 and an inner container 15, a gap is formed between the shell 14 and the inner container 15, and the shell 14 is provided with an inlet 16 for constant temperature medium to enter and an outlet 17 for constant temperature medium to flow out. The water outlet pipe and the water return pipe of the constant temperature circulator 12 are respectively communicated with an inlet 16 and an outlet 17. The inner container 15 is also communicated with a valve g interface 18, a valve h interface 19, a valve i interface 20 and an oxygen concentration detector interface 21.
In this example, the thermostat circulator used was a HX-4008 cryostat. In practical application, the type of the constant temperature circulator is not limited by the above type, and a technician can select a proper type according to specific situations for use.
The high-pressure gas kettle 11 comprises an inner kettle body and an outer temperature control medium jacket, and the constant-temperature circulator 12 is connected with the outer temperature control medium jacket of the high-pressure gas kettle 11 through a pipeline.
The inner layer kettle body is made of hastelloy C276.
The C-276 hastelloy belongs to nickel-molybdenum-chromium-iron-tungsten series nickel base alloy, and is the most corrosion-resistant one of modern metal materials. Mainly resistant to wet chlorine, various oxidizing chlorides, chloride solution, sulfuric acid and oxidizing salts, and has good corrosion resistance in low-temperature and medium-temperature hydrochloric acid. Therefore, the method has quite wide application in harsh corrosive environments, such as chemical industry, petrochemical industry, flue gas desulfurization, paper pulp and papermaking, environmental protection and other industrial fields. The C276 alloy is suitable for various chemical process industries containing oxidation and reduction media, the high molybdenum and chromium contents enable the alloy to resist corrosion of chloride ions, and the tungsten element further improves the corrosion resistance of the alloy. C276 is one of the only materials that can withstand the corrosion of moist chlorine, hypochlorite, and chlorine dioxide solutions, and the alloy has significant corrosion resistance to high-concentration chloride solutions (e.g., ferric chloride and cupric chloride).
The gas loop control system 8 comprises a compressor, gas path switching valves (a, b, c and d) are arranged on pipelines among the compressor, the hydrogen cylinder 5, the nitrogen cylinder 6 and the third gas cylinder 7, and the compressor is connected with an exhaust valve e.
The slow strain rate tensile testing machine 9, the high-pressure gas kettle 11, the gas loop control system 8, the constant-temperature circulator 12, the hydrogen cylinder 5, the nitrogen cylinder 6 and the third type gas cylinder 7 are arranged in a laboratory.
The top in laboratory is equipped with explosion-proof formula frequency conversion air exhauster 2, explosion-proof formula frequency conversion air exhauster 2's control system is connected with baroceptor 1, baroceptor 1 is used for detecting the inside atmospheric pressure in laboratory.
The control system of the explosion-proof variable-frequency exhauster 2 is also connected with a hydrogen concentration detector 3, and the hydrogen concentration detector 3 is used for detecting the concentration of hydrogen in the laboratory.
When the hydrogen detector 3 detects that the concentration of hydrogen in the laboratory reaches a preset threshold value, the control system controls the experiment power supply to be cut off, and meanwhile, the exhaust volume of the explosion-proof variable-frequency exhauster 2 is increased.
In this embodiment, the explosion-proof variable frequency exhauster 2 is EFi120 model 120XX model. In practical application, the type of the explosion-proof variable-frequency exhauster is not limited by the above type, and a person skilled in the art can select a proper type to use according to specific conditions.
The control system of the explosion-proof variable-frequency exhauster 2 is also connected with an alarm 4, and when the hydrogen detector 3 detects that the hydrogen concentration in the laboratory reaches a preset threshold value, the control system controls the alarm 4 to give an alarm.
When the oxygen concentration detector detects that the oxygen concentration in the high-pressure gas kettle exceeds a preset threshold value, the cyclic operation of 'nitrogen purging-nitrogen pressurizing-evacuation exhausting-nitrogen purging' of the high-pressure gas kettle is realized through the process switching of the gas loop control system 8, and the oxygen concentration in the high-pressure gas kettle 11 is reduced.
Example 4
In this embodiment 4, a system for testing hydrogen embrittlement of a material in a high-pressure hydrogen gas and other mixed gas environment for slow tensile and low cycle fatigue (a system for testing hydrogen embrittlement resistance of a material) is provided, as shown in fig. 1, the system includes: a slow strain rate tensile tester 9; a high-pressure gas kettle 11 arranged on the slow strain rate tensile testing machine 9; a hydrogen cylinder 5, a nitrogen cylinder 6 and a third type gas cylinder 7; a gas loop control system 8 connected with the hydrogen cylinder 5, the nitrogen cylinder 6, the third type gas cylinder 7 and the high-pressure gas kettle 11; a high-low temperature constant temperature circulator 12 connected to the high-pressure gas kettle 11 for controlling the temperature of the high-pressure gas kettle 11; an oxygen concentration detector 10 disposed on the high-pressure gas kettle 11; a combustible gas burner 13 connected to the high-pressure gas tank 11; the explosion-proof type variable frequency exhauster 2 is arranged at the top of the laboratory; the device comprises an air pressure sensor 1, a hydrogen concentration detector 3 and an alarm 4, wherein the air pressure sensor 1 is arranged at the top of a laboratory and is connected with an explosion-proof variable-frequency exhauster 2.
In this embodiment 4, the high-pressure gas kettle 11 is installed on the slow strain rate tensile testing machine 9, and includes an inner kettle body and an outer temperature control medium jacket, the inner kettle body is made of hastelloy C276, and can implement high-pressure hydrogen and other gas testing environments at a set temperature.
The slow strain rate tensile testing machine 9 can perform slow strain tensile, low cycle cyclic load fatigue test and constant load creep/stress corrosion test on metal materials, the maximum test force is 50kN, the precision grade is 0.5 grade, and the tensile rate of the slow strain rate tensile testing can be 10-6Stepless regulation between 10mm/min and minimum drawing rate not more than 10-8mm/s。
The gas loop control system 12 is connected with the hydrogen cylinder 5, the nitrogen cylinder 6, the third gas cylinder 7 and the high-pressure gas kettle 11 through pipelines, and the high-pressure gas kettle 11 can be pressurized or vacuumized by using gas in the gas cylinders.
The oxygen concentration detector 10 is installed on the high-pressure gas kettle 11 and used for detecting the oxygen concentration in the high-pressure gas kettle 11, when the oxygen concentration is too high, the gas loop control system 8 is used for nitrogen purging and vacuumizing, the oxygen concentration in the high-pressure gas kettle 11 is guaranteed within a safety range, and explosion danger caused by mixing of hydrogen and oxygen is prevented.
The high-low temperature constant temperature circulator 12 is connected with an outer temperature control medium jacket of the high-pressure gas kettle 11 through a pipeline and is used for controlling the temperature of the high-pressure gas kettle 11, and the temperature control range is-40 ℃ to 200 ℃.
The combustible gas burner 13 is connected with the high-pressure gas kettle 11 through a pipeline, hydrogen-containing waste gas discharged from the high-pressure gas kettle 11 is combusted through the combustible gas burner 13, and water generated by combustion is discharged from a water pipe at the lower part of the combustible gas burner.
The pressure sensor 1 and the explosion-proof type variable frequency exhauster 2 form an explosion-proof type negative pressure variable frequency exhausting system, the explosion-proof type variable frequency exhauster 2 is provided with a control system, and can exhaust according to the pressure measured by the pressure sensor 1 so as to maintain the indoor state of micro negative pressure, and can ensure that the combustible gas is timely exhausted outdoors when trace leakage of the combustible gas occurs.
Atmospheric pressure sensor 1 explosion-proof formula frequency conversion air exhauster 2 hydrogen detector 3 reaches alarm 4 constitutes combustible gas leakage warning and safety control system, control system set up in explosion-proof formula frequency conversion air exhauster 2, when hydrogen detector 3 detected indoor hydrogen concentration and reached certain extreme value, control system control experiment power cuts off, through alarm 4 carries out acousto-optic warning, increases simultaneously 2 air displacement of explosion-proof formula frequency conversion air exhauster.
In practical application, the embodiment 4 is performed according to the following steps:
1. before the experiment, the air tightness of the experimental system device and the pipeline is checked, and the explosion-proof negative pressure variable frequency exhaust system and the combustible gas leakage alarm and safety control system are checked to work normally.
2. And loading a test piece. And clamping the experimental test piece to a clamp of a slow strain rate tensile testing machine 9 in a high-pressure gas kettle 11, sealing the high-pressure gas kettle, and keeping all valves in a closed state.
3. And (5) purging with nitrogen. And (3) opening a gas circuit switching valve b, a gas circuit switching valve f, a valve g, a valve i and a valve in front of the combustible gas combustor 13 in sequence, opening a regulating valve behind the nitrogen cylinder 6, keeping the nitrogen purging system for 10min, closing the valve i, and opening a compressor in the gas loop control system 8 to enable the pressure in the high-pressure gas kettle 11 to reach 1 MPa. And (3) closing the valve b, the valve f and the valve g, opening the valve d, the valve e and the valve h, vacuumizing the high-pressure gas kettle 11 through the compressor at the moment, and discharging gas from an emptying valve behind the valve e. The above steps are repeated until the oxygen concentration detected by the oxygen concentration detector 10 reaches a safe value. And closing the valve h, the valve d and the valve e.
4. Injecting multi-component high-pressure gas. Firstly, opening a valve f and a valve g, then opening a valve a, a valve b and a valve c in turn according to the requirement of the gas partial pressure required by the experiment, enabling each gas in the high-pressure gas kettle 11 to reach the partial pressure required by the experiment through a regulating valve behind the gas cylinder and a compressor in the loop control system 8, and closing all the valves.
5. The high-low temperature constant temperature circulator 12 is opened and the temperature required for the experiment is set. And after the temperature in the high-pressure gas kettle reaches the set temperature, starting to perform slow stretching and low-cycle fatigue experiments according to the experiment requirements.
6. After the loading experiment is finished, the combustible gas combustor 13 and the valve i are opened to slowly discharge the hydrogen-containing waste gas into the combustor for combustion, when the pressure in the high-pressure gas kettle 11 is reduced to normal pressure, the valve b, the valve f and the valve g are opened, nitrogen is adopted for continuously purging until the hydrogen in the high-pressure gas kettle 11 is completely discharged, and the combustible gas combustor 13 is closed. The high-pressure gas kettle 11 is opened, and the experimental test piece is taken out.
In conclusion, the material hydrogen embrittlement resistance test experiment system provided by the embodiment of the invention can be used for performing slow tensile and low cycle fatigue experiments on the hydrogen embrittlement of the material in a multi-component high-pressure gas environment, and can control the experiment temperature and pressure conditions; through the waste gas treatment system, the combustible gas burner carries out combustion treatment on the hydrogen-containing waste gas, and water generated by combustion can be discharged harmlessly; the laboratory environment is maintained in a micro-negative pressure state through the explosion-proof negative pressure variable frequency exhaust system, and the combustible gas can be exhausted outdoors in time due to trace leakage, so that the danger caused by the leakage of the combustible gas is reduced; through combustible gas leakage warning and safety control system, when combustible gas leaks, guarantee personnel and laboratory safety through audible and visual warning, cut off experiment power and increase explosion-proof formula frequency conversion air exhauster displacement, the security of having improved the experiment.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts based on the technical solutions disclosed in the present invention.

Claims (10)

1. The utility model provides a material anti hydrogen embrittlement capability test experimental system which characterized in that includes:
a slow strain rate tensile tester (9);
a high-pressure gas kettle (11) arranged on the slow strain rate tensile testing machine (9); the high-pressure gas kettle (11) is connected with a hydrogen cylinder (5), a nitrogen cylinder (6) and a third type gas cylinder (7) through a gas loop control system (8); injecting the gases in a hydrogen cylinder (5), a nitrogen cylinder (6) and a third gas cylinder (7) into a high-pressure gas kettle (11) at different partial pressures through the gas loop control system (8);
a thermostatic circulator (12) for controlling the temperature of the high-pressure gas kettle (11);
an oxygen concentration detector (10) for detecting the oxygen concentration inside the high-pressure gas kettle (11);
a burner (13) for burning the hydrogen-containing waste gas discharged from the high-pressure gas tank (11).
2. The experimental system for testing the hydrogen embrittlement resistance of materials according to claim 1, wherein the high-pressure gas kettle (11) comprises an inner kettle body and an outer temperature control medium jacket, and the constant-temperature circulator (12) is connected with the outer temperature control medium jacket of the high-pressure gas kettle (11) through a pipeline.
3. The material hydrogen embrittlement resistance test experiment system of claim 2, wherein the inner kettle body is made of hastelloy C276.
4. The test system for testing hydrogen embrittlement resistance of materials according to claim 1,
the gas loop control system (8) comprises a compressor, the compressor is connected with the hydrogen cylinder (5), the nitrogen cylinder (6) and the third type gas cylinder (7) through pipelines, gas path switching valves are arranged on the pipelines, and the compressor is connected with an exhaust valve.
5. The experimental system for testing hydrogen embrittlement resistance of materials according to claim 1, wherein the slow strain rate tensile testing machine (9), the high pressure gas kettle (11), the gas loop control system (8), the constant temperature circulator (12), the hydrogen gas cylinder (5), the nitrogen gas cylinder (6) and the third type gas cylinder (7) are arranged in a laboratory.
6. The experimental system for testing the hydrogen embrittlement resistance of the material according to claim 5, wherein an explosion-proof variable frequency exhauster (2) is arranged at the top of the laboratory, a control system of the explosion-proof variable frequency exhauster (2) is connected with an air pressure sensor (1), and the air pressure sensor (1) is used for detecting air pressure inside the laboratory.
7. The experiment system for testing the hydrogen embrittlement resistance of the material according to claim 6, wherein a control system of the explosion-proof variable frequency exhauster (2) is further connected with a hydrogen concentration detector (3), and the hydrogen concentration detector (3) is used for detecting the concentration of hydrogen in the laboratory.
8. The experiment system for testing the hydrogen embrittlement resistance of the material, according to claim 7, is characterized in that when the hydrogen detector (3) detects that the hydrogen concentration in the laboratory reaches a preset threshold value, the control system controls the experiment power supply to be cut off, and simultaneously increases the exhaust volume of the explosion-proof variable-frequency exhauster (2).
9. The material hydrogen embrittlement resistance performance test experiment system according to claim 7, wherein a control system of the explosion-proof type variable frequency exhauster (2) is further connected with an alarm (4), and when the hydrogen detector (3) detects that the hydrogen concentration in the laboratory reaches a preset threshold value, the control system controls the alarm (4) to give an alarm.
10. The experimental system for testing hydrogen embrittlement resistance of materials, according to claim 1, is characterized in that when the oxygen concentration detector detects that the oxygen concentration in the high-pressure gas kettle exceeds a preset threshold, the cyclic operation of 'nitrogen purging, nitrogen pressurizing, evacuation and exhaust, and nitrogen purging' of the high-pressure gas kettle is realized through the flow switching of the gas loop control system (8), so that the oxygen concentration in the high-pressure gas kettle (11) is reduced.
CN202110768665.7A 2021-07-07 2021-07-07 Experimental system for testing hydrogen brittleness resistance and service life of material in high-pressure hydrogen environment Pending CN113466427A (en)

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CN117110106B (en) * 2023-10-23 2023-12-19 中铝材料应用研究院有限公司 Method for testing fatigue performance of aluminum alloy material in simulated high-pressure hydrogen environment
CN117110053B (en) * 2023-10-23 2023-12-19 中铝材料应用研究院有限公司 Method for testing hydrogen embrittlement sensitivity of aluminum alloy material in simulated high-pressure hydrogen environment

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