CN102323308A - Device and method for researching hydrogen permeation behavior of metal subjected to dead-load pulling stress in gaseous medium - Google Patents
Device and method for researching hydrogen permeation behavior of metal subjected to dead-load pulling stress in gaseous medium Download PDFInfo
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Abstract
The invention relates to a device and method for researching the metallic hydrogen permeation behavior, in particular to a device and method for researching the hydrogen permeation behavior of metal subjected to dead-load pulling stress in a gaseous medium, and the device and method are used for researching the interactive influence of pulling stress and a gaseous environment on the metallic hydrogen permeation behavior. The device comprises a heating device, a stretching device, an electrolytic bath and a liquid/gas storage bottle. The method comprises the steps of: nickel-plating a single side of a test piece to be tested, and fixing the test piece between a lower opening of an anode pool and an upper opening of an environmental pool, wherein the nickel-plated layer of the test piece faces the environmental pool; and providing dead-load pulling stress for the test piece by the stretching device. An experimental medium in the anode pool is a NaOH solution. An experimental solution in the environmental pool forms a gaseous medium environment under the action of water bath. The device and method provided by the invention can be used for researching the hydrogen permeation behavior of a metallic material subjected to dead-load pulling stress in the gaseous medium, the control of the magnitude of the pulling stress and the environment and atmosphere can be realized, and the deficiency that the influence of a stressed state and the gaseous environment on the metallic hydrogen permeation behavior cannot be measured through the traditional electrolytic bath is made up.
Description
Technical field
The present invention relates to study the device and method of metallic hydrogen permeability behavior, specifically a kind of research metal under static tension condition, the device and method of hydrogen permeation behavior in gaseous medium.
Background technology
The behavior of hydrogen embrittlement type stress corrosion crack is the factor that metal has a strong impact on material safety property when in atmospheric environment, being on active service.The interior hydrogen that metal material absorbs in processes such as thermal treatment, pickling, plating and welding and with atmospheric environment in sour gas such as H
2S, SO
2Or CO
2The outer hydrogen that perhaps under the cathodic protection condition, penetrates in the metallic matrix Deng contact all can cause the toughness reduction of sensitive metal material and the degradation of physics or chemical property, influences its military service security.Especially metal material is receiving under the tension condition, and hydrogen more easily and material production reciprocation and the hydrogen embrittlement of atarting material.
Undoubtedly, in gaseous medium, the hydrogen permeation behavior that is in the metal of tensile stress state has determined the stress corrosion opening cracking maleate sensitivity of metal to a great extent.Therefore, be necessary to study metal in gaseous medium, the hydrogen permeation behavior under the static load stretching condition, and research drawing stress and gas especially sour gas to the reciprocal effect of metallic hydrogen permeability behavior.
The hydrogen penetration testing of metal current is mainly based on the two-sided electrolytic cell principle of Devanathan-Stachurski, and existing double-electrolyzer adopts both sides to be the liquid hydrogen permeability apparatus of solution more, is difficult to realize measuring under the gaseous state condition purpose of hydrogen infiltration electric current.In addition, the static load tension does not have the apparatus and method of rational evaluation at present to the influence of Gaseous Hydrogen permeability behavior yet.
Summary of the invention
In order to overcome the deficiency of present method, the purpose of this invention is to provide the device and method of the metal hydrogen permeation behavior in gaseous medium under a kind of suitable research static load tension condition to the research hydrogen permeation behavior.
The object of the invention is realized through following technical scheme.
The present invention is the device of metal hydrogen permeation behavior in gaseous medium under a kind of static load tension condition; Comprise heating arrangement (1), stretching device, electrolytic cell and liquid storage/gas cylinder (21); Described heating arrangement (1) is a thermostat water bath; The interior temperature in pond (10) that is used to control environment, described stretching device is made up of back up pad (3), support column (4) and stretching titanium alloy rod (6), and back up pad (3) is connected by bolt (22) with support column (4); Stretching titanium stretching rod (6) passes back up pad (3) center and is prevented to move forward and backward by firm nut (22); The static load tension is provided by the firm nut of precession (5) holddown spring (7), and the precession distance determines that by the required tension size that adds described electrolytic cell comprises anode pond (8) and anode pond loam cake (9), environment pond (10) and environment pond loam cake (11) according to Hooke's law.Be connected fastening between anode pond (8) and anode pond loam cake (9), environment pond (10) and environment pond loam cake (11), anode pond (8) and environment pond (10) respectively with bolt; Anode pond loam cake (9) is positioned at upper end, anode pond (8); Environment pond loam cake (11) is positioned at environment pond (10) upper end, and (8) lower end, anode pond and environment pond (10) upper end such as all have at big concentric circle holes (12), is provided with auxiliary electrode jack (23) on the anode pond loam cake (9) in the center; The next door is provided with reference electrode reference electrode plug (24); Environment pond (10) has air intake opening (15) and gas outlet (16), and seam crossing is coated with envelope with silica gel, and sample, contrast electrode and auxiliary electrode constitute three-electrode system; And draw lead respectively and link to each other with the corresponding port of data acquisition unit; Described liquid storage/gas cylinder (21) is connected with environment pond (10) through acidproof silicone tube (20), and storage liquid storage/gas cylinder (21) upper end has air intake opening (17), gas outlet (18) and (19) with the plug sealing on the plug; Sample (2) passes electrolytic cell and active section is inner at electrolytic cell, and the inoperative section in the electrolytic cell outside can be connected on the stretching device through bolt (22).
A kind of method that adopts metal device of hydrogen permeation behavior in gaseous medium under the described research static load of the claim 1 tension condition; Sample is fixed between anode pond (8) lower port and environment pond (10) lower port; And whole electrolytic cell is installed on the stretching device; And apply certain stress to sample, and in anode pond (8), pour the NaOH solution of 0.1 mol/L into, it is stable to apply 0.3V constant potential to aftercurrent to sample; Be pressed into environment pond (10) behind experimental solutions deoxygenation 2 h in liquid storage/gas cylinder (21); Make environment pond (10) form the gaseous atmosphere of certain humiture by thermostat water bath (1) heating, measure the sample infiltration of the hydrogen in gaseous atmosphere electric current under static load tension condition, its concrete steps are:
1) with sample with No. 1000 sand paperings after nickel plating, nickel-plating liquid is 250 g/L nickelous sulfate (NiSO
46H
2O), 45 g/L nickel chloride (NiCl
2), 40 g/L boric acid (H
3BO
4) mixed liquor.Sample is used alcohol wash after the nickel plating, and cold wind dries up, and is fixed between the upper opening of lower openings and environment pond (10) in anode pond (8), and seam crossing is coated with envelope with silica gel;
2) the sample two ends are connected on 2 titanium alloy stretching rods (6) of stretching device together with electrolytic cell, and through precession nut (5) holddown spring (7) stress application, the size that adds stress according to need is confirmed the distance of advancing of nut;
3) pour the NaOH solution of 0.1 mol/L into anode pond (8), the degree of depth is not as the criterion can there not to be auxiliary electrode (13) and contrast electrode (14).Anode pond loam cake (9) and anode pond (10) that will be fixed with auxiliary electrode (13) and contrast electrode (14) are sealed.Three electrodes in the anode pond (8) link to each other with data acquisition system (DAS) through lead, and it is stable to apply 0.3 V constant potential to aftercurrent for sample (2); 4) when carrying out step (4), feed N by the air intake opening (17) of liquid storage/gas cylinder (21)
2, close gas outlet (19) and carry out deoxygenation 2 h.Treat that opening gas outlet (19) after step (4) finishes closes (18), N simultaneously
2The experimental solutions of removing peroxide in liquid storage/gas cylinder (21) is pressed onto in the environment pond (10), thereby water bath heat preservation forms the gaseous atmosphere of a constant temperature, humidity in environment pond (10).If directly use sour gas, then directly feed from inlet port (15) as environment pond atmosphere.With data acquisition system (DAS) record hydrogen infiltration electric current in time.
Compared with prior art, of the present invention having the following advantages:
(1) the present invention provides a cover to be fit to the proving installation and the method for metal hydrogen permeation behavior in gaseous medium under the research static load tension condition, has remedied the deficiency that existing electrolytic cell can not be tested the hydrogen permeation behavior of stressed sample in the gaseous environment.
(2) device that the present invention adopted can be realized sample continuous recording hydrogen infiltration electric current under the different tension conditions; And can apply different potentials to sample through the anode pond, can the synthetic study stress intensity, current potential and different pH acidic atmosphere be to the influence of metallic hydrogen infiltration electric current.
(3) device that the present invention adopted establishes one's own system, and except that the data collection, does not need other coordinative composition of equipments to use, and simple to operate, precision is high, can reflect the hydrogen infiltration change in current of very small amount.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is the vertical view of stretching device.
Fig. 3 is the electrolyser construction synoptic diagram.
1. thermostat water baths among the figure; 2. sample; 3. back up pad; 4. support column; 5. clamp nut; 6. titanium alloy stretching rod; 7. spring; 8. anode pond; 9. anode pond loam cake; 10. environment pond; 11. environment pond loam cake; 12. electrolytic cell opening; 13. auxiliary electrode; 14. contrast electrode; 15. feed liquor/gas port; 16. gas outlet; 17. air intake opening; 18. gas outlet; 19. gas outlet; 20. acidproof silicone tube; 21. liquid storage/gas cylinder; 22. bolt; 23. auxiliary electrode socket; 24. contrast electrode socket.
Embodiment
The present invention includes heating arrangement, stretching device, electrolytic cell and liquid storage/gas cylinder (21).Fig. 1 is a structural representation of the present invention.Back up pad of the stretching device among Fig. 2 (3) and support column (4) are selected plow-steel for use, and stretching rod (6) is selected the titanium alloy of acid-fast alkali-proof corrosion for use.Anode pond (8) among Fig. 3 and anode pond loam cake (9), environment pond (10) and environment pond loam cake (11) all adopt acid and alkali-resistance, high temperature resistant organic glass to make.
Back up pad among Fig. 2 in the stretching device (3) and support column (4) link through 4 bolts (21), and 2 titanium alloy stretching rods (6) are inserted in the hole of back up pad (3), and there is screw thread at the two ends of stretching outside, prevent to move forward and backward through firm nut (5).The material of spring is a manganese alloy, can holddown spring (7) during the firm nut of precession (5) thus to sample tension is provided.
As shown in Figure 3, electrolytic cell comprises anode pond (8) and anode pond loam cake (9), environment pond (10) and environment pond loam cake (11).Anode pond loam cake (9) is positioned at upper end, anode pond (8), and environment pond loam cake (11) is positioned at upper end, environment pond (10), uses 4 bolts (22) to connect respectively; The upper end of the lower end in anode pond (8) and environment pond (10) such as has at big concentric circle holes (12), insert sample (2) back between the two with 4 bolts (22) connection, so the two connects into complete electrolytic cell.With silica gel seam crossing is coated with envelope simultaneously.2 ends that stretch that sample stretches out electrolytic cell are connected through bolt (22) with titanium alloy stretching rod (6), and then stretching device and electrolytic cell link together.
Center on the anode pond loam cake (9) is provided with auxiliary electrode jack (23); 1 cm place, next door is provided with reference electrode reference electrode plug (24); Auxiliary electrode (13) and contrast electrode (14) be patchhole (23) and (24) respectively; And with extending into inside, anode pond behind the silica gel sealing, anode pond loam cake (9) can freely take off, and is convenient to pour into solution.Sample (2) is formed three-electrode system as working electrode, and three electrodes are drawn lead and linked to each other with the data acquisition unit corresponding port.
As depicted in figs. 1 and 2, sample (2) is the sheet sample, and center section is an active section, and two ends are the inoperative section.Active section is fixed between anode pond (8) and environment pond (10) and contacts with atmosphere up and down.The single face nickel plating of sample active section, and nickel plating face is towards the environment pond.
Liquid storage bottle/gas cylinder (21) links to each other with the air intake opening (15) of bottom, environment pond (10) through acidproof silicone tube (20), for the environment pond provides acid solution or gas.Can feed N from air intake opening (17) during the experimental solutions deoxygenation
2, open gas outlet (18) and with its water seal, and close gas outlet (19).Feed gas if desired, then directly feed from the air intake opening (15) of environment pond (10).
Electrolytic cell among Fig. 3 is installed on the stretching device shown in Figure 2, and precession clamp nut (5) applies drawing stress to sample (2).The distance of nut precession is determined by required tension.The NaCl solution of in anode pond (8), pouring 0.1 mol/L into is connected to the corresponding port of data collector as medium with three electrodes, and applies 0.3 V constant potential to remove original interior hydrogen in the sample for sample (2), and the test hydrogen-separating quantity over time.Open simultaneously gas outlet (18) and water seal it, close gas outlet (19), feed N from air intake opening (17)
2To remove the O in the solution in liquid storage/gas cylinder (21)
2Close air intake opening (17) and gas outlet (18) behind deoxygenation 2 h.After the interior hydrogen amount of separating out reaches stationary value, open air intake opening (17) and feed N
2Solution in liquid storage bottle/gas cylinder (21) is pressed onto in the environment pond (10).With the air atmosphere of thermostat water bath (1) heating environment pond (10) with the protection stationary temperature.Record liberation of hydrogen electric current is curve over time, and after hydrogen atom reached the stable state diffusion, the liberation of hydrogen electric current reached maximal value, stops record data, finished experiment.
After experiment finishes electrolytic cell is taken off from stretching device, and takes off loam cake (9), pour out the NaOH solution in anode pond (8), the solution in environment pond (10) from the gas outlet (15) pour out and reclaim.Carefully take off sample (2) and spend the ionized water flushing immediately, put into drying basin after cold wind dries up.Then electrolytic cell is cleaned and dried.
Sample is of a size of long 140 mm, wide 22 mm, thickness 0.5mm among the present invention; Sample with No. 1000 sand paperings after, (nickel-plating liquid is 250 g/L nickelous sulfate [NiSO in single face nickel plating
46H
2O], 45 g/L nickel chloride [NiCl
2], 40 g/L boric acid [H
3BO
4] mixed liquor).Filling nitrogen atmosphere is 0.5 mol/L H
2SO
4+ 0.25 g/L As
2O
3The gaseous environment that solution forms under water-bath also can be sour gas such as H
2S, SO
2Or CO
2Environment.
Claims (2)
1. the device of metal hydrogen permeation behavior in gaseous medium under the static load tension; It is characterized in that: comprise heating arrangement (1), stretching device, electrolytic cell and liquid storage/gas cylinder (21); Described heating arrangement (1) is a thermostat water bath, the interior temperature in pond (10) that is used to control environment, and described stretching device is made up of back up pad (3), support column (4) and stretching titanium alloy rod (6); Back up pad (3) is connected by bolt (21) with support column (4); Stretching titanium stretching rod (6) passes back up pad (3) center and is prevented to move forward and backward by firm nut (22), and the static load tension is provided by the firm nut of precession (5) holddown spring (7), and the precession distance is determined by the required tension size that adds according to Hooke's law; Described electrolytic cell comprises anode pond (8) and anode pond loam cake (9), environment pond (10) and environment pond loam cake (11); Be connected fasteningly between anode pond (8) and loam cake (9), environment pond (10) and environment pond loam cake (11), anode pond (8) and environment pond (10) respectively with bolt, anode pond loam cake (9) is positioned at upper end, anode pond (8), and environment pond loam cake (11) is positioned at upper end, environment pond (10); (8) lower end, anode pond and environment pond (10) upper end such as all has at big concentric circle holes (12); Anode pond loam cake (9) is gone up and is provided with auxiliary electrode jack (23) in the center, and the next door is provided with reference electrode reference electrode plug (24), and environment pond (10) have air intake opening (15) and gas outlet (16); Seam crossing is coated with envelope with silica gel; Sample, contrast electrode and auxiliary electrode constitute three-electrode system, and draw lead respectively and link to each other with the corresponding port of data acquisition unit, and described liquid storage/gas cylinder (21) is connected with environment pond (10) through acidproof silicone tube (20); Storage liquid storage/gas cylinder (21) upper end seals with plug; Have air intake opening (17), gas outlet (18) and (19) on the plug, sample (2) passes electrolytic cell and active section is inner at electrolytic cell, and the inoperative section in the electrolytic cell outside is connected on the stretching device through bolt (22).
2. method that adopts metal device of hydrogen permeation behavior in gaseous medium under the described static load tension of claim 1; It is characterized by: sample is fixed between anode pond (8) lower port and environment pond (10) lower port; And whole electrolytic cell is installed on the stretching device; And apply certain stress to sample, and in anode pond (8), pour the NaOH solution of 0.1 mol/L into, it is stable to apply 0.3V constant potential to aftercurrent to sample; Be pressed into environment pond (10) behind experimental solutions deoxygenation 2 h in liquid storage/gas cylinder (21); Make environment pond (10) form the gaseous atmosphere of certain humiture by thermostat water bath (1) heating, measure the sample infiltration of the hydrogen in gaseous atmosphere electric current under static load tension condition, its concrete steps are:
1) with sample with No. 1000 sand paperings after nickel plating, nickel-plating liquid is the mixed liquor of 250 g/L nickelous sulfates, 45 g/L nickel chlorides, 40 g/L boric acid;
Sample is used alcohol wash after the nickel plating, and cold wind dries up, and is fixed between the upper opening of lower openings and environment pond (10) in anode pond (8), and seam crossing is coated with envelope with silica gel;
2) the sample two ends are connected on 2 titanium alloy stretching rods (6) of stretching device together with electrolytic cell, and through precession nut (5) holddown spring (7) stress application, the size that adds stress according to need is confirmed the distance of advancing of nut;
3) pour the NaOH solution of 0.1 mol/L into anode pond (8), the degree of depth is not as the criterion can there not to be auxiliary electrode (13) and contrast electrode (14);
Anode pond loam cake (9) and anode pond (10) that will be fixed with auxiliary electrode (13) and contrast electrode (14) are sealed;
Three electrodes in the anode pond (8) link to each other with data acquisition system (DAS) through lead, and it is stable to apply 0.3 V constant potential to aftercurrent for sample (2);
4) when carrying out step (4), feed N by the air intake opening (17) of liquid storage/gas cylinder (21)
2, close gas outlet (19) and carry out deoxygenation 2 h; Treat to open gas outlet (19) after step (4) finishes, close (18) simultaneously, N
2The experimental solutions of removing peroxide in liquid storage/gas cylinder (21) is pressed onto in the environment pond (10), thereby water bath heat preservation forms the gaseous atmosphere of a constant temperature, humidity in environment pond (10); If directly use sour gas, then directly feed from inlet port (15) as environment pond atmosphere;
With data acquisition system (DAS) record hydrogen infiltration electric current curve over time, when the hydrogen atom diffusion reached stable state, the liberation of hydrogen electric current reached maximal value, stops record, and experiment finishes.
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