CN110954586A - In-situ hydrogen display detection device and detection method - Google Patents
In-situ hydrogen display detection device and detection method Download PDFInfo
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- CN110954586A CN110954586A CN201911307087.6A CN201911307087A CN110954586A CN 110954586 A CN110954586 A CN 110954586A CN 201911307087 A CN201911307087 A CN 201911307087A CN 110954586 A CN110954586 A CN 110954586A
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Abstract
The invention discloses an in-situ hydrogen display detection device and a detection method. The in-situ hydrogen display detection device comprises a first box body, a second box body, a constant current instrument and a heating mechanism, wherein a box cover is arranged at the top of the first box body, a first air inlet and a first air outlet are formed in the box cover, a first opening is formed in the bottom of the first box body, and a metal platinum sheet is arranged in the first box body; the second box body is arranged at the bottom of the first box body and is detachably connected with the first box body, the bottom of the second box body is provided with a liquid inlet and a second gas outlet, the top of the second box body is provided with a second port which is arranged opposite to the first opening, and the opening edge of the second port and the opening edge of the first opening are arranged at intervals; the anode of the constant current instrument is electrically connected with the metal platinum sheet, and the cathode of the constant current instrument is used for being connected with the metal to be detected; the heating mechanism is used for providing heat for the second box body. The invention can carry out electrochemical hydrogen charging on different metals so as to facilitate in-situ detection of the influence of microscopic defects in the metals on hydrogen capture.
Description
Technical Field
The invention relates to the technical field of electrochemical experiments, in particular to an in-situ hydrogen display detection device and a detection method.
Background
When a metal material, particularly a steel material, is in service in an acidic environment, hydrogen enters a steel matrix due to the interaction of the material and the hydrogen. The hydrogen atoms entering the material can be captured and enriched at the microstructure defects of the material, and the mechanical property of the material is reduced due to the existence of the hydrogen, even Hydrogen Induced Cracking (HIC) is initiated, so that the material fails. The influence rule and mechanism of the microstructure defect of the metal material on hydrogen capture are explored, so that the safety of the service of the material is improved, and the economic loss is reduced.
A common method for researching the influence of hydrogen on a metal material is to simulate the interaction of hydrogen and the material, explore the influence factors of hydrogen on the material and disclose the mechanism of the influence factors. In the experiment, hydrogen atoms are introduced into the material in an electrochemical hydrogen charging mode, so that the microstructure of the material and the interaction between inclusions and hydrogen are explored, and the HIC mechanism is disclosed.
The interaction between the microstructure of the metal material and the inclusion and hydrogen is researched, and the currently adopted method is to measure the permeation kinetic curve of hydrogen in the material and then to speculate the influence of the microstructure of the material on hydrogen capture according to the hydrogen permeation kinetic curve, but the position of hydrogen in the microscopic defect of the material cannot be visually observed. HIC failures of steel are generally caused by permeation, diffusion and accumulation of hydrogen, and the accumulation of hydrogen at the microstructure defects of the metal material can be visually observed through hydrogen display experiments.
The hydrogen developing technology is a technology which is developed on the basis of the traditional photographic developing technology and can visually reflect the hydrogen distribution. The principle is that Ag < + > (silver ions) are reduced into white Ag (silver) particles by H through the redox reaction of Ag < + > and H, the particles are distributed at the positions where hydrogen is diffused and captured, and the distribution condition of Ag and silver on the metal surface can be observed through a high-power scanning electron microscope.
The conventional hydrogen display test method is to test the metal to be detected after the hydrogen charging is finished. During the hydrogen charging process, hydrogen atoms in the material can be combined into hydrogen molecules to overflow, and the accuracy of the experimental result is influenced. In addition, in order to ensure the hydrogen concentration during the hydrogen display test, the metal to be detected is generally charged with hydrogen for a long time, and the surface of the metal to be detected is damaged in the process, so that the result is deviated. The in-situ hydrogen display test can ensure higher hydrogen concentration at the test part, reduce the hydrogen charging time and avoid the overflow of hydrogen from the surface of the detected metal. Therefore, the hydrogen display test is carried out while the metal to be detected is charged with hydrogen, which is very beneficial to researching the influence of the internal microscopic defects of the material on hydrogen capture.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide an in-situ hydrogen display detection apparatus and a detection method thereof, which aim to solve the problems of inaccurate detection result, long detection time, waste of hydrogen display agent, etc. of the conventional hydrogen display apparatus.
In order to achieve the above object, the present invention provides an in-situ hydrogen display detection device, comprising:
the device comprises a first box body, a second box body and a third box body, wherein a box cover is arranged at the top of the first box body, a first air inlet and a first air outlet are formed in the box cover, a first opening is formed in the bottom of the first box body, and a metal platinum sheet is arranged in the first box body;
the second box body is arranged at the bottom of the first box body and is detachably connected with the first box body, a liquid inlet and a second gas outlet are formed in the bottom of the second box body, a second port opposite to the first opening is formed in the top of the second box body, and a port edge of the second port and a port edge of the first opening are arranged at intervals to define a placing area for placing the metal to be detected;
the anode of the constant current instrument is electrically connected with the metal platinum sheet, and the cathode of the constant current instrument is used for being connected with the metal to be detected; and the number of the first and second groups,
and the heating mechanism is used for providing heat for the second box body.
Optionally, the lateral wall of the second box extends outwards along the horizontal direction and is provided with a mounting arm, the mounting arm is provided with a mounting hole, the first box corresponds to the mounting hole and is provided with a stud, and the first box and the second box penetrate through a screw and are arranged in the stud and the mounting hole for connection.
Optionally, first air inlet first gas outlet with liquid inlet department all is connected with the connecting pipe, the connecting pipe pass through 703 silica gel with first air inlet first gas outlet with the liquid inlet is connected.
Optionally, the surface of the platinum sheet is opposite to the first opening.
Optionally, the first box and the second box are both arranged in a cylindrical shape, and the first box and the second box are coaxially arranged.
Optionally, the first box body is made of organic glass, and the second box body is made of a PVP light-insulating plastic pipe.
Optionally, the heating mechanism includes a water bath, and a mounting structure is arranged at a mouth of the water bath and used for fixing the first box body to the water bath, so that the second box body and the metal to be detected are accommodated in the water bath.
Optionally, the mounting structure comprises a screen plate, the screen plate is arranged at a pot opening of the water bath, and a plurality of through holes distributed along the circumferential direction are formed in the screen plate.
Optionally, the bottom of the first box is provided with a plurality of protrusions corresponding to the plurality of through holes, and the plurality of protrusions and the plurality of through holes are in one-to-one correspondence and are arranged in a matched manner.
The invention also provides an in-situ hydrogen display detection method, which comprises the following steps:
inputting a hydrogen display solution into the in-situ hydrogen display detection device;
starting the water bath kettle, setting the water temperature to be 60 ℃, installing the first box body on the installation structure, and then preserving heat for 15 min;
inputting a hydrogen filling solution into the in-situ hydrogen display detection device, and continuously introducing nitrogen into the in-situ hydrogen display detection device after the hydrogen filling solution submerges the metal platinum sheet;
starting a constant current meter, setting constant current, starting charging hydrogen, and setting current and charging hydrogen time according to the type of the metal to be detected;
after the hydrogen filling is finished, continuously preserving the heat for 30min, taking out the metal to be detected, cleaning with distilled water and drying;
and observing the metal to be detected by using a scanning electron microscope.
According to the technical scheme, the hydrogen-charging device is provided with the first box body for containing a hydrogen-charging solution, the second box body for containing a hydrogen-displaying solution, a metal to be detected is placed at a connecting opening of the first box body and the second box body, current is applied through a constant current instrument, hydrogen is generated on the hydrogen-charging side of the metal to be detected, interaction between the hydrogen and the metal is simulated, hydrogen diffused to the hydrogen-displaying side of the metal to be detected is oxidized by the hydrogen-displaying solution, Ag particles of the hydrogen-displaying solution are reduced, distribution of Ag is observed through a high-power scanning electron microscope, distribution of the hydrogen is known, detection results are more accurate, and influences of metal microscopic defects on hydrogen capture can be conveniently known through detection of different metals.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an in-situ hydrogen display detection apparatus according to an embodiment of the present invention;
fig. 2 is a schematic structural view of the mounting structure shown in fig. 1.
The reference numbers illustrate:
| reference numerals | Name (R) | Reference numerals | Name (R) |
| 100 | In-situ hydrogen |
22 | |
| 1 | |
23 | |
| 11 | |
3 | Constant |
| 12 | First air outlet | 4 | |
| 13 | First opening hole | 41 | |
| 14 | Protrusion | 42 | |
| 15 | |
421 | |
| 16 | |
422 | Through |
| 2 | |
5 | Metal to be detected |
| 21 | Liquid inlet |
The object of the present invention, its functional characteristics and advantageous effects will be further described with reference to the following embodiments and drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In view of the above, the present invention provides an in-situ hydrogen display detection apparatus and a detection method thereof, and fig. 1 to 2 illustrate embodiments of the in-situ hydrogen display detection apparatus according to the present invention.
Referring to fig. 1, in the present embodiment, the in-situ hydrogen display detection apparatus 100 includes a first box 1, a second box 2, a constant current meter 3 and a heating mechanism 4, where the first box 1 is used for containing a hydrogen filling solution, a box cover is disposed at the top of the first box 1, a first air inlet 11 and a first air outlet 12 are disposed on the box cover, a first opening 13 is disposed at the bottom of the first box 1, a metal 5 to be detected is attached to the first opening 13 for detection, and a metal platinum sheet 15 is disposed in the first box 1; the second box body 2 is used for containing a hydrogen display solution, the second box body 2 is arranged at the bottom of the first box body 1, the second box body 2 is detachably connected with the first box body 1, a liquid inlet 21 is formed in the bottom of the second box body 2, a second port opposite to the first opening 13 is formed in the top of the second box body 2, and a port edge of the second port and a port edge of the first opening 13 are arranged at intervals to define a placing area for placing a metal 5 to be detected; the anode of the constant current instrument 3 is electrically connected with the metal platinum sheet 15, and the cathode is used for being connected with the metal 5 to be detected; the heating mechanism 4 is used for heating the second box body 2.
According to the technical scheme, the first box body 1 is used for containing a hydrogen charging solution, the second box body 2 is used for containing a hydrogen display solution, the metal 5 to be detected is placed at the connecting opening of the first box body 1 and the second box body 2, current is applied through the constant current instrument 3, hydrogen is generated on the hydrogen charging side of the metal to be detected, interaction between the hydrogen and the metal is simulated, the hydrogen displayed solution diffuses to the hydrogen display side of the metal to be detected, Ag particles are reduced, distribution of Ag is observed through a high-power scanning electron microscope, distribution of the hydrogen is known, and influence of micro defects in the metal on hydrogen capture is conveniently known through detection of different metals.
The outer side wall of the second box body 2 extends outwards along the horizontal direction to be provided with an installation arm 23, the installation arm 23 is provided with an installation hole, the first box body 1 corresponds to the installation hole is provided with a stud 16, and the first box body 1 and the second box body 2 are arranged in a penetrating mode through a screw in the stud 16 and the installation hole to be connected. When the metal 5 to be detected is placed, the first box body 1 is detached firstly, the metal 5 to be detected is adhered to the first opening 13 and sealed, the second box body 2 is installed on the first box body 1 through a screw, and the distance between the second box body 2 and the first box body 1 is adjusted through the screw, so that the metal 5 to be detected is tightly pressed by the second box body 2, and the metal 5 to be detected and the second box body 2 can be further sealed through 704 silica gel, so that the metal 5 to be detected and the second box body 2 are well sealed, and the hydrogen-developing solution in the second box body 2 is prevented from overflowing to the second port. Obviously, the connection mode of the first box 1 and the second box 2 is not limited to the above one, and the connection mode of the first box 1 and the second box 2 for installing the metal 5 to be detected should belong to the protection scope of the present application.
In this embodiment, the bottom of the second box 2 may be provided with a liquid outlet 22, the second box 2 may be installed on the first box 1, and then the second box 2 may be filled with hydrogen solution, when the solution overflows from the second gas outlet 22, it indicates that the solution in the second box 2 is full, the liquid inlet and the second gas outlet are sealed by a small rubber plug, and then the second box 2 filled with the solution is placed in the heating mechanism 4. Of course, the manner of entering the hydrogen developing solution is not limited to the above-mentioned one, and the manner of filling the second box 2 so that the metal 5 to be detected can be contacted with the hydrogen developing solution is within the protection scope of the present application.
In this embodiment, first air inlet 11 first gas outlet 12 with liquid inlet 21 department all is connected with the connecting pipe, each the connecting pipe pass through 703 silica gel with first air inlet 11 first gas outlet 12 liquid inlet 21 with liquid outlet 22 is connected, bonds and seals through silica gel, and is sealed effectual, and easily dismantles.
In this embodiment, the metal platinum sheet is used for electrically connecting with the constant current meter 3, and when the surface of the metal platinum sheet 15 is disposed opposite to the first opening 13, that is, the metal platinum sheet 15 is generally disposed in a sheet shape, and when the sheet surface of the metal platinum sheet 15 is opposite to the first opening 13, the current distribution is optimal.
In this embodiment, the first box 1 and the second box 2 are both cylindrical, and the first box 1 and the second box 2 are coaxial.
The material of first box 1 sets up to organic glass to whether the hydrogen solution of observing in the first box 1 has the submergence metal platinum piece 15, the material of second box 2 sets up to PVP light-proof plastic tubing, guarantees that hydrogen shows the dark surrounds of in-process.
The heating mechanism 4 comprises a water bath 41, a mounting structure 42 is arranged at a pot opening of the water bath 41, and the mounting structure 42 is used for fixing the first box body 1 on the water bath 41, so that the second box body 2 and the metal 5 to be detected are arranged in a water body in the water bath 41. The first box body 1 is placed in the water bath 41, the second box body 2 and the metal 5 to be detected are immersed in the water body of the water bath 41, and the water level of the water body in the water bath 41 is just equal to that of the metal 5 to be detected, so that the hydrogen-developing solution is heated.
Further, referring to fig. 2, the mounting structure 42 includes a screen 421, the screen 421 is disposed at the pot opening of the water bath 41, an annular mounting table is disposed on an inner side wall of the pot opening, the screen 421 is mounted on the annular mounting table, and a plurality of through holes 422 arranged along the circumferential direction are disposed on the screen 421, so that the first box 1 and the second box 2 are mounted on the screen 421.
Further, the bottom of the first box 1 is provided with a plurality of protrusions 14 corresponding to the plurality of through holes 422, the plurality of protrusions 14 and the plurality of through holes 422 are matched in a one-to-one correspondence manner, when the first box is installed, the plurality of protrusions 14 are inserted into the plurality of through holes 422, so that the first box 1 can be installed on the water bath 41, and the installation is convenient.
In the present embodiment, the first air inlet 11 of the first tank 1 is communicated with a hydrogen charging solution tank; the liquid inlet 21 of the second box body 2 is communicated with a hydrogen display solution tank so as to conveniently add a hydrogen charging solution into the first box body 1 and add a hydrogen display solution into the second box body 2, thus the detection is more convenient. And pouring the deoxygenated hydrogen-filled solution into the first box body 1 from the first air inlet 11, wherein the liquid level of the solution is higher than 5 pieces of metal platinum. And (3) injecting a hydrogen-developing solution into the second box body 2 from the liquid inlet 21 by using a dropper, and blocking the liquid inlet 21 and the second air outlet 22 by using a small rubber plug when the solution overflows from the liquid outlet 22.
The invention also provides an in-situ hydrogen display detection method for hydrogen display detection by the in-situ hydrogen display detection device, which specifically comprises the following steps:
inputting a hydrogen display solution into the in-situ hydrogen display detection device;
starting the water bath kettle, setting the water temperature to be 60 ℃, and keeping the temperature for 15 min;
inputting a hydrogen filling solution into the in-situ hydrogen display detection device, and continuously introducing nitrogen into the in-situ hydrogen display detection device after the hydrogen filling solution submerges the metal platinum sheet;
starting a constant current meter, setting constant current, starting charging hydrogen, and setting current and charging hydrogen time according to the type of the metal to be detected;
after the hydrogen filling is finished, continuously preserving the heat for 30min, taking out the metal to be detected, and cleaning and drying the metal by distilled water;
and observing the metal to be detected by using a scanning electron microscope.
The in-situ hydrogen evolution test of the X70 pipeline steel is specifically described as follows:
1. the metal 5 to be tested was ground and polished with a sheet-like X70 pipeline steel of dimensions 30X 20X 1.5 mm. And (3) inverting the first box body 1, adhering the metal 5 to be detected to the first opening 13 under the hydrogen charging chamber by using 704 silica gel, and fully covering the first opening 13 by using the metal 5 to be detected. And bonding the copper wire to one side of the metal 5 to be detected by using the conductive paster. And (3) inversely placing the second box body 2 on the metal 5 to be detected, and bonding and sealing the second box body with 704 silica gel. The central axis of the first box body 1 and the central axis of the second box body 2 are ensured to be on the same straight line. The metal 5 to be detected is sealed integrally by 704 silica gel, so that no electricity leakage is ensured.
2. After the silica gel is completely solidified, injecting a hydrogen-developing solution into the second box body 2 from the liquid inlet 21 by using a dropper, when the solution overflows from the liquid outlet 22, indicating that the second box body 2 is filled with the solution, and sealing the liquid inlet 21 and the second air outlet 22 by using a small rubber plug. In the embodiment, the hydrogen charging solution is prepared by using a mixed solution containing 1g of AgBr nuclear latex and 3mL of 1.4mol/L sodium nitrite in a dark place.
3. And placing the first box body 1 containing the metal 5 to be detected and the second box body 2 on a screen plate of a water bath kettle, and installing through an installation structure. And the liquid level of the water in the water bath kettle is just equal to the metal 5 to be detected, and the water bath temperature is set to be 60 ℃.
4. Keeping the temperature for 15min, and after the solution in the second box body 2 reaches 60 ℃, pouring the hydrogen-filled solution after oxygen removal into the first box body 1 through the first air inlet 11, wherein the liquid level of the solution is higher than the metal platinum sheet 15. In this case, the hydrogen-charged solution contains 0.5mol/L sulfuric acid and 3.1X 10-3And (3) a mixed solution of mol/L sodium pyrophosphate.
5. And (3) connecting a copper wire connected with the metal platinum sheet 15 into the anode of the constant current instrument, and connecting a copper wire connected with the metal 5 to be detected into the cathode of the constant current instrument. And nitrogen is continuously introduced from the first gas outlet 12, so that an oxygen-free environment in the hydrogen filling process is ensured. Opening the constant current instrument and setting the constant current to be 30mA/cm2And starting to charge hydrogen for 10 min.
6. And after the hydrogen filling is finished, keeping the temperature for 30min to ensure that the H diffused to one side of the hydrogen display chamber completely reacts with Ag +.
7. And (5) after the heat preservation is finished, removing the 704 silica gel, taking out the metal 5 to be detected, cleaning with distilled water and drying. And finally moving to a scanning electron microscope for observation.
In conclusion, the hydrogen-in-situ hydrogen-display test device is novel in design, simple in structure, convenient and fast to use, saves hydrogen-display reagents, can be used for performing in-situ hydrogen-display test on the metal 5 to be detected after being charged with hydrogen, and is suitable for a test for observing hydrogen distribution at a microscopic defect in the metal.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structures made by using the contents of the specification and the drawings of the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. An in-situ hydrogen display detection device, comprising:
the device comprises a first box body, a second box body and a third box body, wherein a box cover is arranged at the top of the first box body, a first air inlet and a first air outlet are formed in the box cover, a first opening is formed in the bottom of the first box body, and a metal platinum sheet is arranged in the first box body;
the second box body is arranged at the bottom of the first box body and is detachably connected with the first box body, a liquid inlet and a second gas outlet are formed in the bottom of the second box body, a second port opposite to the first opening is formed in the top of the second box body, and a port edge of the second port and a port edge of the first opening are arranged at intervals to define a placing area for placing the metal to be detected;
the anode of the constant current instrument is electrically connected with the metal platinum sheet, and the cathode of the constant current instrument is used for being connected with the metal to be detected; and the number of the first and second groups,
and the heating mechanism is used for providing heat for the second box body.
2. The in-situ hydrogen display detection device according to claim 1, wherein an installation arm extends outwards from an outer side wall of the second box body along a horizontal direction, the installation arm is provided with an installation hole, a stud is arranged at a position, corresponding to the installation hole, of the first box body, and the first box body and the second box body are connected by penetrating through the stud and the installation hole through screws.
3. The in-situ hydrogen display detection device according to claim 1, wherein the first air inlet, the first air outlet and the liquid inlet are connected with connecting pipes, and each connecting pipe is connected with the first air inlet, the first air outlet and the liquid inlet through 703 silica gel.
4. The in-situ hydrogen display detection device according to claim 1, wherein a surface of the platinum sheet is disposed opposite to the first opening.
5. The in-situ hydrogen display detection device according to claim 1, wherein the first box and the second box are both arranged in a cylindrical shape, and the first box and the second box are coaxially arranged.
6. The in-situ hydrogen display detection device according to claim 1, wherein the first box body is made of organic glass, and the second box body is made of PVP light-proof plastic tube.
7. The in-situ hydrogen display detection device according to claim 1, wherein the heating mechanism comprises a water bath, and a mounting structure is arranged at a pot opening of the water bath and used for fixing the first box body and the metal to be detected on the water bath so that the second box body is immersed in the water bath.
8. The in-situ hydrogen display detection device according to claim 6, wherein the mounting structure comprises a screen plate, the screen plate is arranged at the pot mouth of the water bath pot, and a plurality of through holes are arranged on the screen plate along the circumferential direction.
9. The in-situ hydrogen display detection device according to claim 7, wherein a plurality of protrusions are disposed at the bottom of the first box body and correspond to the plurality of through holes, and the plurality of protrusions and the plurality of through holes are disposed in a one-to-one corresponding manner.
10. An in-situ hydrogen display detection method is characterized by comprising the following steps:
inputting a hydrogen display solution into a second box body of the in-situ hydrogen display detection device;
starting the water bath kettle, setting the water temperature to be 60 ℃, installing the first box body on the installation structure, and then preserving heat for 15 min;
inputting a hydrogen filling solution into a first box body of the in-situ hydrogen display detection device, and continuously introducing nitrogen into the first box body of the in-situ hydrogen display detection device after the hydrogen filling solution submerges a metal platinum sheet;
starting a constant current instrument, starting charging hydrogen, and setting current and charging hydrogen time according to the type of the metal to be detected;
after the hydrogen filling is finished, continuously preserving the heat for 30min, taking out the metal to be detected, cleaning with distilled water and drying;
and observing the metal to be detected by using a scanning electron microscope.
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| CN107607561A (en) * | 2017-10-17 | 2018-01-19 | 新余钢铁股份有限公司 | A kind of detection means of hydrogen storage vessel workpiece hydrogen defect |
| CN113092205A (en) * | 2021-03-30 | 2021-07-09 | 北京科技大学 | Simple hydrogen micro-printing method for detecting hydrogen distribution in metal |
| CN113186547A (en) * | 2021-04-19 | 2021-07-30 | 武汉科技大学 | Method and device for efficiently preparing high-purity high-pressure hydrogen by utilizing scrap steel |
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