CN106226167B - Test device for measuring hydrogen brittleness resistance of metal sample under variable prestress condition - Google Patents
Test device for measuring hydrogen brittleness resistance of metal sample under variable prestress condition Download PDFInfo
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- CN106226167B CN106226167B CN201610654202.7A CN201610654202A CN106226167B CN 106226167 B CN106226167 B CN 106226167B CN 201610654202 A CN201610654202 A CN 201610654202A CN 106226167 B CN106226167 B CN 106226167B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/20—Investigating strength properties of solid materials by application of mechanical stress by applying steady bending forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/04—Chucks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0236—Other environments
- G01N2203/024—Corrosive
Abstract
The invention relates to the field of materials and electrochemistry, in particular to a test device for measuring hydrogen embrittlement resistance of a metal sample under a variable prestress condition, which comprises a sample clamping device, a mechanical loading system, a motor control system, a stress sensor, a temperature control system and an air expelling system; the test for measuring the influence of different stress change rate conditions on the hydrogen embrittlement resistance of the sample is realized, the electrochemical hydrogen charging of the series circuit is adopted to reduce the test period of multiple samples, the test efficiency is improved, the stability of the medium is maintained by introducing the temperature control system and the gas driving system, and the precision of the hydrogen embrittlement test is improved.
Description
Technical Field
The invention relates to the field of materials science and electrochemistry, in particular to an electrochemical hydrogen charging device adopting a series circuit, wherein a motor loading system is added in the device, so that a hydrogen embrittlement test of a sample under the conditions of different stress change rates is realized, the test period of multiple samples is shortened, and the test efficiency is improved; the introduction of the temperature control system and the gas driving system maintains the stability of the medium and improves the precision of the hydrogen embrittlement test.
Background
The pipeline steel belongs to high-strength low-alloy steel, has higher mechanical strength and good toughness at normal temperature, and is widely applied to the transportation of petroleum and natural gas. The conveying pipeline is mostly in a humid environment, the conveying medium contains hydrogen sulfide and acidic substances, and cathodic protection is mostly adopted, atomic hydrogen generated by hydrogen evolution reaction diffuses into steel in the protection process, so that cavities are formed at crystal boundaries, hydrogen bubbling, hydrogen induced cracking and sulfide stress corrosion cracking are caused, and the mechanical property is greatly degraded. Hydrogen is the root cause of various pipeline breakage accidents and becomes one of the hidden dangers threatening the safe operation of pipelines. In other fields, such as steel making, welding, moisture is reduced at high temperature to generate hydrogen and dissolved in liquid metal; or when the equipment is used for electroplating or pickling, the surface of the steel is supersaturated with the adsorbed hydrogen atoms, so that the hydrogen permeates into the steel. The hydrogen embrittlement hidden danger exists in various metal workpieces generally, the material can be subjected to sudden brittle fracture to cause serious accidents, and the hydrogen embrittlement hidden danger has great significance for research on hydrogen embrittlement behaviors. The electrochemical hydrogen permeation method is considered as a classical method for studying the diffusion behavior of hydrogen in metals.
The conventional hydrogen charging device adopts a single-wire hydrogen charging device, which is schematically shown in FIG. 1, that is, only one sample and platinum sheet are arranged on each line. The hydrogen charging method has certain advantages, such as large hydrogen charging amount, simple test operation, easy control of main influencing factors such as current, temperature and the like. However, for the hydrogen embrittlement test with a large sample demand, the single-line hydrogen charging is bound to store the sample which is firstly charged with hydrogen, and the subsequent experimental observation is carried out after the group of samples are charged with hydrogen, so that the period for completing the group of hydrogen embrittlement tests is long, hydrogen can hardly escape in the process of storing liquid nitrogen, and the influence of the measurement variable prestress condition on the hydrogen embrittlement resistance of the sample is difficult to meet.
Disclosure of Invention
In order to solve the problems, the invention provides a test device for measuring the hydrogen embrittlement resistance of a metal sample under a variable prestress condition, which comprises an electrolytic cell, a sample clamping device, a mechanical loading system, a motor control system, a stress sensor, a data acquisition unit and a temperature control system; the test for measuring the influence of different stress change rate conditions on the hydrogen embrittlement resistance of the sample is realized, the electrochemical hydrogen charging of the series circuit is adopted to reduce the test period of multiple samples, the test efficiency is improved, the stability of the medium is maintained by introducing the temperature control system and the gas driving system, and the precision of the hydrogen embrittlement test is improved.
The technical scheme is as follows:
the method comprises the steps of carrying out single-side nickel plating on a metal sheet sample by adopting a watt plating solution, then clamping the sample by using a sample clamping device, wherein the sample clamping device mainly comprises a clamp body, a fastening bolt and a sealing device, the sample is arranged in clamping grooves at two ends of the clamp body, the end surfaces of the clamping grooves are in a right trapezoid shape, the included angle between the trapezoid inclined edge and the vertical surface of the sample is 40 degrees so as to ensure that the sample cannot pop up in the bending process, the clamp body is made of nickel-based alloy so as to meet the high bearing capacity and the corrosion resistance of the clamp body, and is fixed on the inner side of an electrolytic tank through the fastening bolt, and.
Bending stress is applied to the sample through a mechanical loading system, and the relation between the loading speed and the stress change rate of the sample is measured. The mechanical loading system mainly comprises a motor, a ball screw, a push rod and a sealing rubber film; the motor is connected with the ball screw, the ball screw is driven to run by the motor, the push rod is connected with a moving block in the ball screw, the push rod sequentially penetrates through a sealing device of a sample clamping device arranged on the side wall of the electrolytic cell and a clamp body to be contacted with a sample, the moving block drives the push rod to advance and applies bending stress to the sample, the motor rotates forwards and backwards to control the stroke direction of the push rod, the motor selects a small gear reduction motor 6IK300RGU, the push rod is made of nickel-based alloy, and the size of the push rod is 20 multiplied by 6 mm; the different stroke speeds of the ball screw are realized by controlling the different loading speeds of the motor through a motor control system, so that the different stress change rates of the samples are realized; the contact position of the push rod and the sample is sealed by a rubber film, so that the leakage of electrolyte in the loading process is avoided; and a stress sensor is arranged at the central position of the sample, is connected with the data acquisition unit and records the stress change rate of the sample corresponding to different loading speeds.
Adjusting the sample and a loading device to recover the initial state, then adopting a series circuit to carry out electrochemical hydrogen charging, connecting N samples and platinum sheet electrodes corresponding to the number of the electrolytic tanks in series in one loop, namely connecting the anode of a regulated power supply (1) with the platinum sheet electrode in a first electrolytic tank, connecting the cathode sample with the platinum sheet electrode in a second electrolytic tank through a lead, connecting the cathode sample in the second electrolytic tank with the platinum sheet electrode in a third electrolytic tank, connecting the cathode sample in the third electrolytic tank with the platinum sheet electrode in a fourth electrolytic tank until the cathode sample in the N electrolytic tank is connected with the cathode of the regulated power supply, adding 0.1mol/L NaOH solution and 1.26mol/L Na solution into the electrolytic tanks4P2O7The liquid level of the poisoning agent is based on the fact that the liquid level can submerge the sample and the platinum electrode, and normal pressure N is introduced into the electrolytic bath2The oxygen-expelling treatment is carried out, and the length, the width and the height of the electrolytic bath are respectively 300mm, 200mm and 200 mm.
The electrolytic bath is positioned in the thermostatic bath, the thermostatic device is opened to allow the thermostatic medium to flow into the thermostatic bath from the water inlet and return from the water outlet, and the control of the temperature of the thermostatic bath is realized by controlling the water inlet throttle valve and the water outlet throttle valve.
When the dissolved oxygen content in the electrolyte solution is reduced to the specified requirement, the stabilized voltage power supply is adjusted to stabilize the hydrogen charging current at 0.07A, then the required motor speed is set according to the stress change relation of the sample corresponding to the loading speed obtained by the data acquisition unit, so that the samples in the electrolytic cell respectively obtain the stress change rate required by the test, and the reciprocating motion of the ball screw is controlled through the positive and negative rotation of the motor, so that the cyclic reciprocation of the stress change of the samples is realized, and a continuous stress change process is obtained.
After about 140 hours of electrolytic hydrogen charging treatment, the stabilized voltage power supply is closed, the sample is taken out, the sample is placed in an ultrasonic cleaning machine, an alcohol solution is used for washing away a surface electrolyte solution, and after air drying, hydrogen embrittlement cracks on the surface of the sample are observed by using a scanning electron microscope.
The invention has the beneficial effects that: the invention provides a set of test device for detecting the hydrogen embrittlement resistance of a metal material under the variable prestress condition, which is suitable for multiple samples, and overcomes the defects that the conventional hydrogen embrittlement test device has long test period and low efficiency and cannot measure the influence of the variable prestress on the hydrogen embrittlement resistance of the metal material; the introduction of the temperature control system and the gas driving system maintains the stability of the medium and improves the precision of the hydrogen embrittlement test.
Drawings
FIG. 1 is a schematic diagram of the structure of the novel hydrogen embrittlement test device of the invention.
Fig. 2 is a schematic structural diagram of the novel sample holding device and the loading device of the present invention.
FIG. 3 is a surface topography of a sample after the novel hydrogen embrittlement test of the invention.
In the figure: 1. the device comprises a voltage-stabilized power supply, 2, a data acquisition unit, 3, a motor, 4, a ball screw, 5, a fastening bolt, 6, a platinum electrode, 7, a water inlet throttle valve, 8, a constant temperature device, 9, a stress sensor, 10, an electrolytic bath, 11, a constant temperature bath, 12, a sample, 13, a motor control system, 14, a sample clamping device, 15, a screw rod rubber gasket, 16, a water outlet rubber gasket, 17, a water outlet, 18, a water outlet throttle valve, 19, a clamp body, 20, a fastening bolt, 21, a sealing device, 22, a sealing rubber film and 23, and a push rod.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
The utility model provides a measure test device of anti hydrogen embrittlement ability of metal specimen under variable prestressing force condition, includes sample clamping device, mechanical loading system, motor control system, stress sensor, temperature control system and drives the gas system. The test for measuring the influence of different stress change rate conditions on the hydrogen embrittlement resistance of the sample is realized, the electrochemical hydrogen charging of the series circuit is adopted to reduce the test period of multiple samples, the test efficiency is improved, the stability of the medium is maintained by introducing the temperature control system and the gas driving system, and the precision of the hydrogen embrittlement test is improved.
Selecting AZ31B magnesium alloy as a research object, preparing the magnesium alloy into 20mm multiplied by 5mm multiplied by 2mm slices, dividing all samples into three groups, each group comprises two samples, and setting motor parameters to sequentially increase the stress change rate.
The method comprises the steps of carrying out single-side nickel plating on a metal sheet sample 12 by adopting a watt plating solution, then clamping the sample 12 by using a clamping device, wherein the clamping device 14 mainly comprises a clamp body 19, a fastening bolt 20 and a sealing device 21, the sample is installed in clamping grooves at two ends of the clamp body 19, the end surfaces of the clamping grooves are in a right trapezoid shape, the included angle between the inclined edge of the trapezoid and the vertical surface of the sample is 40 degrees so as to ensure that the sample cannot pop up in the bending process, the clamp body 19 is made of a nickel-based alloy to meet the requirements of high bearing capacity and corrosion resistance of the clamp body, and is fixed on the inner side of an electrolytic tank 10 through the fastening bolt 20.
The ball screw 4 is driven to run by the motor 3, the push rod 23 is connected with a moving block in the ball screw 4, the moving block drives the push rod 23 to advance and apply bending stress to the sample 12, the motor 3 rotates forwards and backwards to control the stroke direction of the push rod 23, the motor 3 selects a small gear reduction motor 6IK300RGU, and the push rod 23 is made of nickel-based alloy and has the size of 20 multiplied by 6 mm; the motor control system 13 controls the difference of the loading speeds of the three motors 3 to realize the difference of the advancing speeds of the ball screw 4, so that the difference of the stress change rates of the samples 12 is realized, and the contact part of the push rod 23 and the samples 12 is sealed by a rubber film 22 to avoid the leakage of electrolyte in the loading process; and a stress sensor 9 is arranged at the center of the sample 24, the stress sensor 9 is connected with the data acquisition unit 2, and the stress change rates of the sample corresponding to different loading speeds are recorded.
Adjusting the sample and a loading device to recover the initial state, then adopting a series circuit to carry out electrochemical hydrogen charging, connecting 3 samples and a platinum sheet electrode in series in a loop, namely connecting the anode of a stabilized voltage power supply 1 with a platinum electrode 6 in a first electrolytic tank, connecting a cathode sample with the platinum electrode 6 in a second electrolytic tank through a lead, connecting the cathode sample in the second electrolytic tank with the platinum electrode 6 in a third electrolytic tank, connecting the cathode sample in the third electrolytic tank with the cathode of the stabilized voltage power supply 1, adding 0.1mol/L NaOH solution and 1.26mol/L Na solution into an electrolytic tank 104P2O7The liquid level of the poisoning agent is based on the level of the sample 12 and the platinum electrode 6, and normal pressure N is introduced into the electrolytic cell2And performing oxygen-expelling treatment.
The thermostat 8 is opened to let the thermostatic medium flow from the inlet into the thermostatic bath 11 and back from the outlet, and the control of the thermostatic bath temperature is achieved by controlling the inlet throttle valve 7 and the outlet throttle valve 18. When the dissolved oxygen content in the electrolyte solution is reduced to the specified requirement, the stabilized voltage power supply 1 is adjusted to stabilize the hydrogen charging current at 0.07A, then the required motor speeds are set according to the stress change relation of the sample corresponding to the loading speed obtained by the data collector 2, which are respectively 4r/min, 8r/min and 16r/min, so that the samples in the three electrolytic tanks respectively obtain the stress change rate required by the test, and the reciprocating motion of the ball screw 4 is controlled through the positive and negative rotation of the motor 3, so as to realize the cyclic reciprocation of the stress change of the sample, namely obtain a continuous stress change process.
After about 140 hours of electrolytic hydrogen charging treatment, the power supply is turned off, the sample is taken out, the sample is placed in an ultrasonic cleaning machine, the surface electrolyte solution is washed away by using an alcohol solution, and after air drying, the hydrogen embrittlement cracks on the surface of the sample are observed by using a scanning electron microscope, as shown in fig. 3.
In the embodiment, under the same hydrogen charging current and temperature, the influence of the variable prestress condition on the hydrogen embrittlement resistance of the magnesium alloy material is measured, the test time is greatly shortened, the test result is accurate, and the surface morphology of the sample after the hydrogen embrittlement test can be seen as follows: the faster the stress changes, the easier it is for cracks to initiate, and the width as well as the length of the crack increase significantly.
Claims (5)
1. The utility model provides a measure test device of anti hydrogen embrittlement ability of metal specimen under variable prestressing force condition which characterized in that: the testing device comprises an electrolytic cell (10), a sample clamping device (14), a mechanical loading system, a motor control system (13), a stress sensor (9), a data acquisition unit (2) and a temperature control system, wherein the electrolytic cell (10), the sample clamping device (14), the mechanical loading system and the stress sensor (9) are the same in number;
the method comprises the following steps of carrying out single-side nickel plating on a metal sheet sample (12) by adopting a watt plating solution, then clamping the sample (12) by using a sample clamping device, wherein the sample clamping device (14) mainly comprises a clamp body (19), a fastening bolt (20) and a sealing device (21), the sample is arranged in clamping grooves at two ends of the clamp body (19), and the clamp body (19) is fixed on the inner side of an electrolytic bath (10) through the fastening bolt (20);
applying bending stress to the sample through a mechanical loading system, and measuring the relation between the loading speed and the stress change rate of the sample; the mechanical loading system mainly comprises a motor (3), a ball screw (4), a push rod (23) and a sealing rubber film (22); the motor (3) is connected with the ball screw (4), the ball screw (4) is driven to operate through the motor (3), the push rod (23) is connected with a moving block in the ball screw (4), the push rod (23) sequentially penetrates through a sealing device (21) and a clamp body (19) of a sample clamping device (14) arranged on the side wall of the electrolytic cell to be contacted with a sample, the moving block drives the push rod (23) to advance and apply bending stress to the sample (12), the motor (3) controls the stroke direction of the push rod in a forward and reverse rotation mode, the different stroke speeds of the ball screw (4) are realized by controlling the different loading speeds of the motor (3) through the motor control system (13), and therefore the different stress change rates of the sample are realized; the contact part of the push rod (23) and the test sample (12) is sealed by a sealing rubber film (22), so that the leakage of electrolyte in the loading process is avoided; a stress sensor (9) is arranged at the center of the sample (12), the stress sensor (9) is connected with the data acquisition unit (2), and the stress change rates of the sample corresponding to different loading speeds are recorded;
adjusting the samples and a loading device to restore the initial state, and then carrying out electrochemical hydrogen charging by adopting a series circuit, wherein N samples (12) and platinum electrodes (6) corresponding to the number of the electrolytic cells (10) are connected in series in one loop, namely, the anode of a stabilized voltage power supply (1) is connected with the platinum electrode (6) in the first electrolytic cell, the cathode sample (12) is connected with the platinum electrode (6) in the second electrolytic cell through a lead, similarly, the cathode sample (12) in the second electrolytic cell is connected with the platinum electrode (6) in the third electrolytic cell, the cathode sample (12) in the third electrolytic cell is connected with the platinum electrode (6) in the fourth electrolytic cell until the cathode sample (12) in the N electrolytic cell is connected with the cathode of the stabilized voltage power supply (1);
the electrolytic bath (10) is positioned in the thermostatic bath (11), the thermostatic device (8) is opened to allow a thermostatic medium to flow into the thermostatic bath (11) from the water inlet and return from the water outlet, and the temperature of the thermostatic bath is controlled by controlling the water inlet throttle valve (7) and the water outlet throttle valve (18).
2. The test device for measuring the hydrogen embrittlement resistance of the metal test sample under the variable pre-stress condition as claimed in claim 1, wherein: the end faces of the clamping grooves at the two ends of the fixture body (19) are right trapezoid, and the included angle between the trapezoid inclined edge and the vertical surface of the sample (12) is 40 degrees so as to ensure that the sample cannot be popped up in the bending process.
3. The test device for measuring the hydrogen embrittlement resistance of the metal test sample under the variable pre-stress condition as claimed in claim 1, wherein: the motor (3) is a small gear reduction motor 6IK300RGU, and the push rod (23) is made of nickel-based alloy and has the size of 20 multiplied by 6 mm.
4. The test device for measuring the hydrogen embrittlement resistance of the metal test sample under the variable pre-stress condition as claimed in claim 1, wherein: 0.1mol/L NaOH solution and 1.26mol/L Na are added into the electrolytic cell (10)4P2O7The liquid level of the poisoning agent is based on the fact that the sample (12) and the platinum electrode (6) can be submerged, and normal pressure N is introduced into the electrolytic tank (10)2The oxygen-expelling treatment is carried out, and the length, the width and the height of the electrolytic bath (10) are respectively 300mm, 200mm and 200 mm.
5. The test device for measuring the hydrogen embrittlement resistance of the metal test sample under the variable pre-stress condition as claimed in claim 1, wherein: when the content of dissolved oxygen in the electrolyte solution in the electrolytic cell is reduced to the specified requirement, adjusting a stabilized voltage power supply to stabilize the hydrogen charging current at 0.07A, then setting the required motor speed according to the stress change relation of the sample corresponding to the loading speed obtained by a data acquisition unit, enabling the sample in the electrolytic cell to respectively obtain the stress change rate required by the test, and controlling the reciprocating motion of a ball screw through the forward and reverse rotation of the motor to realize the cyclic reciprocation of the stress change of the sample, namely obtaining a continuous stress change process; after about 140 hours of electrolytic hydrogen charging treatment, the stabilized voltage power supply is closed, the sample is taken out, the sample is placed in an ultrasonic cleaning machine, an alcohol solution is used for washing away a surface electrolyte solution, and after air drying, hydrogen embrittlement cracks on the surface of the sample are observed by using a scanning electron microscope.
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