CN108279188A - One kind is for measuring electrochemical hydrogen permeation curve device under tensile load - Google Patents
One kind is for measuring electrochemical hydrogen permeation curve device under tensile load Download PDFInfo
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Abstract
One kind is for measuring electrochemical hydrogen permeation curve device under tensile load, the present invention relates to a kind of measurement electrochemical hydrogen permeation curve devices, the present invention is in order to solve cannot to measure Hydrogen permeation curve of the sample under elastic strain and elastoplasticity synthesis strain in the prior art, it includes drawing mechanism, upper mounted plate, bottom plate, drive screw rod, test specimen, test specimen upper junction plate, test specimen lower connecting plate, first electrolytic cell, second electrolytic cell, computer data collector, electrochemical analyser, strain gauge, constant-current supply cathodic hydrogen charging mechanism, constant-current supply cathodic hydrogen charging platinum electrode, electrochemical analyser calomel electrode and electrochemical analyser platinum electrode;The present invention is used for electrochemical hydrogen permeation fields of measurement.
Description
Technical field
The present invention relates to a kind of measurement electrochemical hydrogen permeation curve devices, and in particular to one kind under tensile load for measuring
Electrochemical hydrogen permeation curve device.
Background technology
The penetration curve that the prior art measures is not bear to obtain under plus load in sample, can only be permeated by measuring
Material is carried out to be stretched to plastic deformation before curve, then discharges load, retains plastic strain part, elastic part can be shunk
It goes back, material is finally processed into the size that infiltration sample needs, can not so measure sample and be moulded in elastic strain and bullet
Property synthesis strain under Hydrogen permeation curve.
Invention content
The present invention is integrated in elastic strain and elastoplasticity under strain to solve to measure sample in the prior art
Hydrogen permeation curve, and then provide a kind of for measuring electrochemical hydrogen permeation curve device under tensile load.
The present invention adopts the technical scheme that in order to solve the above problem:It includes drawing mechanism, upper mounted plate, lower fixation
Plate, driving screw rod, test specimen, test specimen upper junction plate, test specimen lower connecting plate, the first electrolytic cell, the second electrolytic cell, computer data are received
Storage, electrochemical analyser, strain gauge, constant-current supply cathodic hydrogen charging mechanism, constant-current supply cathodic hydrogen charging platinum
Electrode, electrochemical analyser calomel electrode and electrochemical analyser platinum electrode;Test specimen upper junction plate and test specimen lower connecting plate are curved
Plate, test specimen are ' work ' font plate, and one end of test specimen upper junction plate is fixedly mounted on by screw on the upper mounted plate of drawing mechanism,
Test specimen lower connecting plate is fixedly mounted on by screw on the bottom plate of drawing mechanism, test specimen upper junction plate and test specimen lower connecting plate
Between be fixedly connected by test specimen, be respectively equipped with the first electrolytic cell and the second electrolytic cell on the both sides of the face of test specimen, the first electrolysis
Pond and the second electrolytic cell are respectively with respect to mounted on the both sides of test specimen, the hydrogen outlet end pipe of the first electrolytic cell and the second electrolytic cell hydrogen
With the side sealed set of test specimen, computer data collector connect gas entrance end pipe with electrochemical analyser, electrochemical credit
Electrochemical analyser calomel electrode and electrochemical analyser platinum electrode in analyzer are inserted on the second electrolytic cell, and constant-current supply is cloudy
The constant-current supply cathodic hydrogen charging platinum electrode that pole electrolysis is flushed with hydrogen on mechanism anode is inserted on the second electrolytic cell, strain gauge
It is connect with test specimen, electrochemical analyser is connected by a side of circuit and test specimen, another side of test specimen passes through circuit
It is connect with the cathode of constant-current supply cathodic hydrogen charging mechanism.
The beneficial effects of the invention are as follows:
1, the present invention carries out the measurement of electrochemical hydrogen permeation curve under the conditions of plus load, realizes material in hydrogen and answers
Experiment under force coupling action, and then the dehiscence process of quantitative analysis hydrogen induced cracking, are loaded using mechanic jacks, are realized
To the loading procedure of sample.Measuring device size in view of electrochemistry and the size for needing load, select mechanical vertical board
Jack carries out.Magnitude of load suffered by sample, the elongation percentage by measuring sample is converted, therefore is needed by ten thousand before testing
Energy stretching-machine measures the stress-strain diagram of sample.The materials power such as Young's modulus and yield strength is obtained according to stress-strain diagram
Performance parameter is learned, then uses the method for finite element to carry out calculating the stress for being flushed with hydrogen position and strain size, finally determines calibration
Position strains and is flushed with hydrogen the load bearing stress correspondence in position.
2, the present invention measures Hydrogen permeation curve of the test specimen 7 under elastic strain and elasticity and plasticity synthesis deformation, so as to
The hydrogen Penetration Signatures such as hydrogen diffusion coefficient, the hydrogen concentration obtained under load effect are calculated by Hydrogen permeation curve, make experimental condition more
Further close to the actual state that hydrogen diffusion and hydrogen induced cracking are formed in engineering.
3, the first electrolytic cell 8 of the invention is flushed with hydrogen by constant-current supply cathodic hydrogen charging mechanism 13, and then to test specimen 7
It is flushed with hydrogen, according to Fick's law of diffusion to 9 side diffusion of the second electrolytic cell, 7 the first electrolytic cell of side 8 of test specimen is spread the hydrogen in test specimen 7
Hydrogen out is measured by electrochemical analyser, and carries out record hydrogen infiltration electric current at any time by computer software chi600e
Variation.It is calculated by the Hydrogen permeation curve of record and obtains hydrogen diffusion coefficient and hydrogen concentration distribution.
Description of the drawings
Fig. 1 is the overall structure front view of the present invention.
Fig. 2 be upper mounted plate 2, bottom plate 3, driving screw rod 4, test specimen 7, test specimen upper junction plate 5, test specimen lower connecting plate 6,
First electrolytic cell 8 and the second electrolytic cell 9 are mounted on the side view on drawing mechanism 1.
Fig. 3 is the front view of test specimen upper junction plate 5.
The side view of Fig. 4 Fig. 3.
Fig. 5 is the vertical view of Fig. 4.
Fig. 6 is the front view of test specimen lower connecting plate 6.
Fig. 7 is the side view of Fig. 6.
Fig. 8 is the vertical view of Fig. 7.
Fig. 9 is the structure chart of test specimen 7.
Figure 10 is the stress-strain diagram that tensile sample is measured by universal tensile machine, to obtain the mechanical property ginseng of material
Number, wherein abscissa indicate that the strain value unit of tensile sample is (%), and ordinate indicates the corresponding stress value of tensile sample
Unit is (MPa).
Figure 11 is to be flushed with hydrogen position in the Stress distribution obtained according to the progress of test specimen in Fig. 97 finite element simulation calculation to answer
The corresponding diagram of power and mark position strain, wherein abscissa indicate that the strain value unit of foil gauge position is (‰), ordinate table
Show that the stress value unit for being flushed with hydrogen and bearing position is (MPa).
Figure 12 is that the present invention measures electrochemical hydrogen permeation curve schematic device.
Specific implementation mode
Specific implementation mode one:Illustrate present embodiment in conjunction with Fig. 1-Figure 12, it is a kind of for stretching described in present embodiment
Under load measure electrochemical hydrogen permeation curve device, it include drawing mechanism 1, upper mounted plate 2, bottom plate 3, driving screw rod 4,
Test specimen 7, test specimen upper junction plate 5, test specimen lower connecting plate 6, the first electrolytic cell 8, the second electrolytic cell 9, computer data collector 10,
Electrochemical analyser 11, strain gauge 12, constant-current supply cathodic hydrogen charging mechanism 13, constant-current supply cathodic hydrogen charging platinum
Electrode 14, electrochemical analyser calomel electrode 15 and electrochemical analyser platinum electrode 16;It is connected under test specimen upper junction plate 5 and test specimen
Plate 6 is bent plate, and test specimen 7 is ' work ' font plate, and one end of test specimen upper junction plate 5 is fixedly mounted on drawing mechanism 1 by screw
On upper mounted plate, test specimen lower connecting plate 6 is fixedly mounted on by screw on the bottom plate 3 of drawing mechanism 1, test specimen upper junction plate
It is fixedly connected by test specimen 7 between 5 and test specimen lower connecting plate 6,8 He of the first electrolytic cell is respectively equipped on the both sides of the face of test specimen 7
Second electrolytic cell 9, the first electrolytic cell 8 and the second electrolytic cell 9 are respectively with respect to mounted on the both sides of test specimen 7, the hydrogen of the first electrolytic cell 8
Gas export end pipe and 9 hydrogen inlet end pipe of the second electrolytic cell with the side sealed set of test specimen 7, computer data collector 10
It is connect with electrochemical analyser 11, the electrochemical analyser calomel electrode 15 on electrochemical analyser 11 and electrochemical analyser platinum
Electrode 16 is inserted on the second electrolytic cell 9, the constant-current supply catholyte on 13 anode of constant-current supply cathodic hydrogen charging mechanism
It is flushed with hydrogen platinum electrode 14 to be inserted on the second electrolytic cell 9, strain gauge 12 is connect with test specimen 7, and electrochemical analyser 11 passes through line
Road is connect with a side of test specimen 7, another side of test specimen 7 passes through circuit and constant-current supply cathodic hydrogen charging mechanism 13
Cathode connection.
10 model chi600e data collecting systems of present embodiment Computer data collector, 7 thickness of test specimen exist
Between 0.5mm~1.0mm, both side surface polishes and is polished to 1 μm, and test specimen 7 is patch test specimen, and test specimen 7 is close to the first electrolysis
The surface of 8 side of pond carries out Nickel Plating Treatment, and nickel coating thickness is about 0.2 μm, and nickel layer can rapid oxidation under the positive potential of 0.25V
It is covered in surface for one layer of fine and close oxidation film, protects the nickel of internal layer and iron not oxidized.
The length L of test specimen 7 is 170mm in present embodiment, and the width W of test specimen 7 is 60mm, the width of 7 both ends transverse slat of test specimen
Degree A is 23.38mm, and the length H of 7 middle connecting plate of test specimen is 100mm, and 7 middle connecting plate of test specimen is logical with the transverse slat at both ends respectively
It crosses the rounded corner that radius is 12mm to connect, 7 middle connecting plate both sides of test specimen are machined with concave edge, the width of concave edge is machined on test specimen 7
Degree W1 is 24mm, and it is that the first electrolytic cell 8 and second is electrolysed when measuring that the circle at the middle connecting plate of concave edge is machined on test specimen 7
Pond 9 is mounted on the relative position on test specimen 7, close to the rectangular place of circular 42mm is that strain is surveyed on the middle connecting plate of test specimen 7
Measure the strain gauge adhesion position of instrument 12.
Specific implementation mode two:Illustrate present embodiment in conjunction with Fig. 1-Fig. 2, it is a kind of described in present embodiment to be carried for stretching
Electrochemical hydrogen permeation curve device is measured under lotus, it further includes geometrical clamp 18, the hydrogen outlet end pipe and second of the first electrolytic cell 8
9 hydrogen inlet end pipe of electrolytic cell is fixedly mounted on by geometrical clamp 18 on test specimen 7, and test specimen 7 and the first electrolytic cell 8 and second are electrolysed
Pond 9 is fixed by washer and flange seal, the first electrolytic cell 8 and the second electrolytic cell 9 by geometrical clamp 18, other structures with
Specific implementation mode one is identical.
Specific implementation mode three:Illustrate present embodiment in conjunction with Fig. 1-Fig. 2, it is a kind of described in present embodiment to be carried for stretching
Electrochemical hydrogen permeation curve device is measured under lotus, it further includes two springs 17, and two springs 17 are fixed at solid vertically
On fixed board 2 and bottom plate 3, the both ends of each spring 17 are respectively and fixedly installed on upper mounted plate 2 and bottom plate 3, and two
A spring 17 is mounted on test specimen 7 on the drawing mechanism 1 of the opposite other side, to prevent in scissor-like jack loading procedure due to two
Side load is inconsistent and causes jack crooked, is loaded using bilateral, to balance two side loads.It is fixed using dual spring, spring
Both ends hook catch on and be vertically connected with part, other structures are same as the specific embodiment one.
Specific implementation mode four:Illustrate present embodiment in conjunction with Fig. 1-Fig. 2, it is a kind of described in present embodiment to be carried for stretching
Electrochemical hydrogen permeation curve device is measured under lotus, drawing mechanism 1 is scissor-like jack, and upper mounted plate 2 is mounted on scissor-like jack
Top on, bottom plate 3 be mounted on scissor-like jack bottom end on, other structures are identical as specific implementation mode one or three.
Specific implementation mode five:Embodiment is described with reference to Fig. 1, a kind of under tensile load described in present embodiment
Measure electrochemical hydrogen permeation curve device, foil gauge be installed on strain gauge 12, strain gauge 12 by foil gauge with
Test specimen 7 connects, and foil gauge is attached to the centre position that test specimen 7 deforms homogeneity range, ensures the reliable and stable of strain result, and will answer
Become piece to be connected on strain gauge 12.The bolt position for rotating scissor-like jack, is loaded, passes through strain gauge 12
Reading determines the size of strain.Other structures are same as the specific embodiment one.
Specific implementation mode six:Embodiment is described with reference to Fig. 1, a kind of under tensile load described in present embodiment
Measure electrochemical hydrogen permeation curve device, foil gauge be installed on strain gauge 12, strain gauge 12 by foil gauge with
Test specimen 7 connects, and other structures are same as the specific embodiment one.
Specific implementation mode seven:Embodiment is described with reference to Fig. 1, a kind of under tensile load described in present embodiment
Electrochemical hydrogen permeation curve device is measured, test specimen 7 is bolted to connection with test specimen upper junction plate 5, and test specimen 7 connects on test specimen
It is equipped with flat shim close to test specimen 7 at fishplate bar 5, test specimen 7 is bolted to connection with test specimen lower connecting plate 6, test specimen 7 and test specimen
It is equipped with flat shim close to test specimen 7 at lower connecting plate 6, contact area is increased by flat shim, ensures test specimen 7 in loading procedure
Stabilization, other structures are same as the specific embodiment one.
Operation principle
The method of present invention electrochemistry can measure the diffusion coefficient of hydrogen in the material, Study of Hydrogen oozing in a metal
Saturating behavior, tissue and mechanical change of the simulation material under ambient containing hydrogen.Its principle is with double-electrolyzer clamping sheet metal examination
Part 7 is electrolysed in 7 side of test specimen, and using constant-current source as power supply, test specimen 7 is used as cathode, and reduction reaction occurs, and hydrogen ion is reduced into
Hydrogen atom, hydrogen atom some enter test specimen 7 in diffuse to the other side, hydrogen atom in addition is then combined into hydrogen molecule, float
It to electrolyte surface, diffuses in air, cell reaction is happened at 8 side of the first electrolytic cell, is known as being flushed with hydrogen side, hydrogen atom expands
It is dissipated to the sample other side and hydrogen ion is oxidized to by constant positive potential, provide constant positive potential by electrochemical analyser 11, survey simultaneously
Charge and electric current caused by oxidation hydrogen atom are measured, is changed over time by the software records charge and electric current installed on computer
Curve, i.e. hydrogen permeate charge curve and hydrogen permeates current curve, and measuring device schematic diagram is as shown in figure 12, this device contains data
Acquisition system chi600e, the first electrolytic cell 8, the second electrolytic cell 9, electrochemical analyser 11, constant-current source, reference electrode, auxiliary electricity
Pole and test specimen 7 etc..First electrolytic cell 8, the second electrolytic cell 9 divide the left and right sides, i.e., cathode chamber and anode chamber, test specimen 7 are clipped in the middle
Fixed both sides are respectively facing the first electrolytic cell 8 and the second electrolytic cell 9, and with washer and flange seal, cathode chamber Inner electrolysis generates hydrogen
Atom, hydrogen atom can enter test specimen 7, can also be combined into hydrogen molecule, in order to allow the hydrogen atom of greater proportion to enter test specimen 7,
Certain As can be added in the electrolytic solution2O3。
0.5mol/L H are used at room temperature2SO4As electrolyte, 0.25g/L As are added2O3, test specimen is cathode, platinum electrode
For anode.Sample is used as anode again in anode chamber simultaneously, keeps the hydrogen for expanding to 7 this side of test specimen former using the positive potential of 0.25V
Son is fully oxidized to hydrogen ion at once, and the NaOH solution and platinum electrode and calomel electrode of 0.2mol/L are housed in anode chamber.Because
The polarization potential of iron is lower than hydrogen, in order to prevent iron atom from being aoxidized prior to hydrogen atom, plates nickel layer in the side before experiment, nickel layer exists
Under the positive potential of 0.25V can rapid oxidation be one layer of fine and close oxidation film be covered in surface, protect internal layer nickel and iron not by oxygen
Change, plating solution is 250g/L NiSO4·7H2O and 45g/L NiCl2·6H2O and 40g/L H3BO4Mixed solution, referred to as watt
Solution.Electroplating temperature is 12~20 DEG C, current density 10mA/cm2, time 120s.
Test procedure is that the test specimen 7 of single-side nickel-plating is clamped to the first electrolytic cell 8,9 center of the second electrolytic cell, with
After be added solution, anode-side applies 0.25V positive potentials, is deducted back end electric current so that coating surface generates fine and close oxidation
Film, current density are down to 1 μ A/cm2Afterwards, start with certain current density be electrolysed with constant-current source in cathode chamber to be flushed with hydrogen, electricity
The hydrogen atom that solution generates is ionized after diffusing to the sample other side, and the electric current and charge at each moment are remembered by electrochemical analyser
It records and transmits in computer, obtain the transient process curve of charge and electric current about the time.
Claims (7)
1. one kind is for measuring electrochemical hydrogen permeation curve device under tensile load, it is characterised in that:It includes drawing mechanism
(1), upper mounted plate (2), bottom plate (3), driving screw rod (4), test specimen (7), test specimen upper junction plate (5), test specimen lower connecting plate
(6), the first electrolytic cell (8), the second electrolytic cell (9), computer data collector (10), electrochemical analyser (11), strain are surveyed
Measure instrument (12), constant-current supply cathodic hydrogen charging mechanism (13), constant-current supply cathodic hydrogen charging platinum electrode (14), electrochemical credit
Analyzer calomel electrode (15) and electrochemical analyser platinum electrode (16);Test specimen upper junction plate (5) and test specimen lower connecting plate (6) are curved
Plate, test specimen (7) are ' work ' font plate, and one end of test specimen upper junction plate (5) is fixedly mounted on the upper of drawing mechanism (1) by screw
In fixed plate, test specimen lower connecting plate (6) is fixedly mounted on by screw on the bottom plate (3) of drawing mechanism (1), is connected on test specimen
It is fixedly connected by test specimen (7) between fishplate bar (5) and test specimen lower connecting plate (6), is respectively equipped on the both sides of the face of test specimen (7)
One electrolytic cell (8) and the second electrolytic cell (9), the first electrolytic cell (8) and the second electrolytic cell (9) are opposite respectively to be mounted on test specimen (7)
Both sides, the side of the hydrogen outlet end pipe and the second electrolytic cell (9) hydrogen inlet end pipe of the first electrolytic cell (8) with test specimen (7)
Face sealed set, computer data collector (10) are connect with electrochemical analyser (11), the electricity on electrochemical analyser (11)
Chemical analyzer calomel electrode (15) and electrochemical analyser platinum electrode (16) are inserted on the second electrolytic cell (9), constant-current supply
Constant-current supply cathodic hydrogen charging platinum electrode (14) on cathodic hydrogen charging mechanism (13) anode is inserted into the second electrolytic cell (9)
On, strain gauge (12) is connect with test specimen (7), and electrochemical analyser (11) is connected by a side of circuit and test specimen (7)
It connects, another side of test specimen (7) is connect by circuit with the cathode of constant-current supply cathodic hydrogen charging mechanism (13).
2. a kind of for measuring electrochemical hydrogen permeation curve device under tensile load according to claim 1, it is characterised in that:
It further includes geometrical clamp (18), and the hydrogen outlet end pipe and the second electrolytic cell (9) hydrogen inlet end pipe of the first electrolytic cell (8) pass through
Geometrical clamp (18) is fixedly mounted on test specimen (7).
3. a kind of for measuring electrochemical hydrogen permeation curve device under tensile load according to claim 1, it is characterised in that:
It further includes two springs (17), and two springs (17) are fixed at vertically on upper mounted plate (2) and bottom plate (3), often
The both ends of a spring (17) are respectively and fixedly installed on upper mounted plate (2) and bottom plate (3), and two springs (17) are mounted on
With test specimen (7) with respect on the drawing mechanism (1) of the other side.
4. described a kind of for measuring electrochemical hydrogen permeation curve device under tensile load according to claim 1 or 3, feature exists
In:Drawing mechanism (1) is scissor-like jack, and upper mounted plate (2) is mounted on the top of scissor-like jack, bottom plate (3) peace
On the bottom end of scissor-like jack.
5. a kind of for measuring electrochemical hydrogen permeation curve device under tensile load according to claim 1, it is characterised in that:
Foil gauge is installed, strain gauge (12) is connect by foil gauge with test specimen (7) on strain gauge (12).
6. a kind of for measuring electrochemical hydrogen permeation curve device under tensile load according to claim 1, it is characterised in that:
Foil gauge is installed, strain gauge (12) is connect by foil gauge with test specimen (7) on strain gauge (12).
7. a kind of for measuring electrochemical hydrogen permeation curve device under tensile load according to claim 1, it is characterised in that:
Test specimen (7) is bolted to connection with test specimen upper junction plate (5), close to test specimen at test specimen (7) and test specimen upper junction plate (5)
(7) it is equipped with flat shim, test specimen (7) is bolted to connection with test specimen lower connecting plate (6), is connected under test specimen (7) and test specimen
At plate (6) flat shim is equipped with close to test specimen (7).
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