CN110133090B - In-situ hydrogen charging experimental device - Google Patents

In-situ hydrogen charging experimental device Download PDF

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CN110133090B
CN110133090B CN201910555060.2A CN201910555060A CN110133090B CN 110133090 B CN110133090 B CN 110133090B CN 201910555060 A CN201910555060 A CN 201910555060A CN 110133090 B CN110133090 B CN 110133090B
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lower shell
upper cover
cover body
hydrogen charging
hydrogen
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CN110133090A (en
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叶飞
陶平
赵晨宇
巩建鸣
耿鲁阳
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Nanjing Tech University
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Nanjing Tech University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract

The invention discloses an in-situ hydrogen charging experimental device which comprises a base, a lower shell and an upper cover body. The longitudinal section of the lower shell is of a convex structure, the lower shell is fixed on the base through a locking bolt, symmetrically arranged through holes are formed in the lower shell and the upper cover body, and the upper cover body is fixed on the lower shell through a fastening screw. The hollow inner chamber of lower casing is equipped with the indent microscope carrier, and upper cover body center is equipped with the syringe needle test hole, and the syringe needle test hole sets up directly over the microscope carrier. The upper cover body is also provided with a wire connecting hole, two sides of the upper convex part of the lower shell are provided with a pair of bulges, and two sides of the upper cover body are provided with grooves matched with the bulges. The invention has novel structural design and convenient use, and can carry out in-situ hydrogen charging test on a hydrogen charging sample. The invention is suitable for the instruments using probes for measuring such as nano indentation, atomic force microscope and the like.

Description

In-situ hydrogen charging experimental device
Technical Field
The invention relates to the technical field of electrochemical experiments, in particular to an in-situ hydrogen charging experimental device.
Background
Hydrogen has an adverse effect on almost all metals of hydrogen induced plasticity loss and reduced resistance to hydrogen induced cracking, which phenomena are commonly referred to collectively as hydrogen embrittlement. While the material may have hydrogen entering the material during preparation, processing and use. Therefore, research on the effect of hydrogen on materials has become a key to safe and economical use of materials.
In order to study the effect of hydrogen on the material, mechanical testing of the hydrogen containing samples is required. Common methods of charging are aqueous electrolytic charging, molten salt electrolytic charging and gas phase charging, wherein aqueous electrolytic charging is most widely used because of its safety and ease of operation.
Conventional mechanical experiments such as uniaxial stretching experiments and the like can reflect the influence of hydrogen on the material on a macroscopic scale. However, as research proceeds, the effect of hydrogen on materials, especially the effect of hydrogen on different phases of metallic materials, on a microscopic scale is becoming increasingly important. Microscopic scale studies often require the use of tiny probes to determine the area of investigation, such as nanoindentation equipment.
The traditional test method is to take out the sample after hydrogen filling for testing, and hydrogen in the material can be combined into hydrogen to overflow in the interval from the completion of hydrogen filling to the beginning of the test, so that the accuracy of the experimental result is affected; in addition, in order to ensure the hydrogen concentration during the test, the sample is often charged with hydrogen for a long time, which can damage the surface of the sample and is unfavorable for the next test. The in-situ test can ensure that the test part always maintains higher hydrogen concentration, the hydrogen charging time can be reduced, and no hydrogen overflows. Therefore, the continuous online test while the sample is charged with hydrogen is very beneficial to researching the influence of hydrogen on the material.
As described above, the performance test of the microscopic dimension of the material can be realized by the probe-like equipment such as the nanoindentation instrument, but at present, no device for continuously and online testing the sample while charging hydrogen is provided for the equipment, which is insufficient to meet the requirement of researching the hydrogen embrittlement phenomenon of the material on the microscopic dimension at present.
Disclosure of Invention
The invention aims to provide an in-situ hydrogen charging experimental device, which realizes continuous online test of a sample while charging hydrogen so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the in-situ hydrogen charging experimental device comprises a base, a lower shell and an upper cover body, wherein the longitudinal section of the lower shell is of a convex structure, the lower shell is fixed on the base through a locking bolt, symmetrically arranged through holes are formed in the lower shell and the upper cover body, and the upper cover body is fixed on the lower shell through a fastening screw; the center of the lower shell is provided with a cylindrical hollow inner cavity, the hollow inner cavity is provided with a carrying platform, and the height of the carrying platform is lower than the upper edge of the hollow inner cavity; the center of the upper cover body is provided with a needle head test hole, the needle head test hole is arranged right above the carrier, and the upper cover body is also provided with a wire guide hole; protrusions are arranged on two opposite sides of the upper protruding portion of the lower shell, and grooves matched with the protrusions are arranged on two opposite sides of the upper cover body; an outward overflow port is formed in the bulge; the side wall of the upper bulge of the lower shell is provided with a liquid inlet, and the side wall of the opposite side is provided with a liquid outlet; and a rubber sealing gasket is arranged at the joint between the lower shell and the base.
Preferably, the carrier adopts a concave carrier, and the carrier adopts a cylindrical structure.
Preferably, the base, the lower shell and the upper cover are all made of organic glass polymer materials.
The application method of the in-situ hydrogen charging experimental device comprises the following steps:
A. firstly, connecting a liquid inlet on a lower shell with a flow pump through a liquid inlet pipe, and then connecting a liquid outlet with a container through a liquid outlet pipe;
B. placing the round sample welded with the lead on a carrier, directly injecting the hydrogen charging solution into the lower shell through a lead hole by using an injector, and enabling the liquid level to be 1 mm beyond the surface of the sample;
C. putting the platinum counter electrode into hydrogen charging solution through the wire guide hole, and fixing the upper cover body and the lower shell body by using a fastening bolt;
D. connecting a lead and a platinum counter electrode welded on a sample to an electrochemical workstation, and opening the electrochemical workstation according to the current density preset in an experiment;
E. starting a flow pump, feeding the hydrogen charging solution into the lower shell through a liquid inlet by the flow pump, discharging the hydrogen charging solution into an external container from a liquid outlet, and continuously circulating the hydrogen charging solution in the lower shell;
F. and finally, after the liquid level of the hydrogen charging solution is stable, the operation probe enters the needle head test hole to perform experimental operation.
The beneficial effects of the invention are as follows:
(1) The invention has novel structural design and convenient use, and can continuously test the in-situ mechanical properties of the hydrogen-filled sample. The invention is suitable for the instruments using probes for measuring such as nano indentation, atomic force microscope and the like.
(2) The invention adopts the flow pump to renew the charging solution, thereby ensuring that the container has fresh solution and ensuring the charging concentration.
(3) The upper cover body of the invention has a limit function on the probe and protects the safety of the sensor above the probe.
(4) The invention has compact design and can be used normally even if the probe is short.
(5) The invention uses the concave carrier, which not only limits the freedom degree of the round sample, but also ensures the rigidity of the sample, thereby enabling the experiment to be carried out smoothly.
(6) The base, the lower shell and the upper cover body are all made of high polymer materials, and the base, the lower shell and the upper cover body have excellent wear resistance and corrosion resistance, are not easy to damage and have long service life.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Fig. 2 is a schematic view of the lower housing structure of the present invention.
Fig. 3 is a schematic view of the structure of the upper cover of the present invention.
The device comprises a base 1, a lower shell 2, an upper cover 3, a fastening screw 4, a carrying platform 5, a needle head test hole 6, a wire guide 7, a protrusion 8, a groove 9, an overflow port 10, a liquid inlet 11 and a liquid outlet 12.
Fig. 4 is an optical micrograph of 2205 duplex stainless steel before and after charging a for 1 hour, b for 5 hours, and c for 5 hours.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The in-situ hydrogen charging experimental device comprises a base 1, a lower shell 2 and an upper cover body 3, wherein the longitudinal section of the lower shell 2 is of a convex structure, the lower shell 2 is fixed on the base 1 through a locking bolt, symmetrically arranged through holes are formed in the lower shell 2 and the upper cover body 3, the upper cover body 3 is fixed on the lower shell 2 through a fastening screw 4, a cylindrical hollow inner cavity is formed in the center of the lower shell 2, a carrying platform 5 is arranged in the hollow inner cavity, and the height of the carrying platform 5 is lower than the upper edge of the hollow inner cavity; the invention discloses a hydrogen charging device, which is characterized in that an indentation needle testing hole 6 is formed in the center of an upper cover body 3, the indentation needle testing hole 6 is arranged right above a carrying platform 5, a wire connecting hole 7 is formed in the upper cover body 3, protrusions 8 are arranged on two opposite sides of an upper protruding portion of a lower shell 2, grooves 9 matched with the protrusions 8 are formed in two opposite sides of the upper cover body 3, an outward overflow port 10 is formed in the protrusions 8, a liquid inlet 11 is formed in one side of a protruding side wall of the lower shell 2, a liquid outlet 12 is formed in the other opposite side of the protruding side wall of the lower shell 2, the liquid inlet 11 is connected with a flow pump through a liquid inlet pipe, and the liquid outlet 12 is connected with a container through a liquid outlet pipe. A rubber sealing gasket is arranged at the joint between the lower shell 2 and the base 1.
In the invention, the upper cover body 3 plays a limiting role on the probe, and the safety of the sensor above the probe is protected.
In the invention, the carrier 5 adopts a concave carrier, which is lower than the upper edge of the hollow inner cavity, and the carrier 5 adopts a cylinder structure. The invention uses the concave carrier, which limits the freedom degree of the round sample and ensures the rigidity of the sample, thereby the experiment can be carried out smoothly.
In the invention, the base 1, the lower shell 2 and the upper cover 3 are all made of organic glass polymer materials, and the organic glass polymer material has excellent wear resistance and corrosion resistance, is not easy to damage and has long service life.
The application method of the in-situ hydrogen charging experimental device comprises the following steps:
A. firstly, a liquid inlet 11 on a lower shell 2 is connected with a flow pump through a liquid inlet pipe, and a liquid outlet 12 is connected with a container through a liquid outlet pipe;
B. placing the round sample welded with the lead on a carrier 5, directly injecting the hydrogen charging solution into the lower shell 2 by a syringe through a lead hole 7, and enabling the liquid level to exceed the surface of the sample by 1 millimeter;
C. putting a platinum counter electrode into a hydrogen charging solution through a wire guide 7, and fixing the upper cover body 3 and the lower shell 2 by using a fastening screw 4;
D. connecting a lead and a platinum counter electrode welded on a sample to an electrochemical workstation, and opening the electrochemical workstation according to the current density preset in an experiment;
E. starting a flow pump, wherein the flow pump sends the hydrogen charging solution into the lower shell 2 through a liquid inlet 11, and discharges the hydrogen charging solution into an external container through a liquid outlet 12, and the hydrogen charging solution in the lower shell 2 is continuously circulated;
F. finally, after the liquid level of the hydrogen charging solution is stable, the operation probe enters the needle head test hole 6 for experimental operation.
Example 1
Taking an in-situ hydrogen filling test of 2205 duplex stainless steel in a Hysicron company TI-premier nanoindenter as an example, the specific embodiments thereof are as follows:
1. the liquid inlet 11 on the lower shell 2 is connected with a flow pump through a liquid inlet pipe, and the liquid outlet 12 is connected with a solution collecting container through a liquid outlet pipe;
2. placing a 2205 duplex stainless steel round sample which is ground and polished and welded with a wire into a carrier 5, enabling the wire to pass through a wire guide 7, directly injecting a hydrogen charging solution into a lower shell 2 by using an injector, enabling the liquid level to exceed the surface of the sample by 1 millimeter, wherein the hydrogen charging solution in the example is a mixed solution containing 0.5mol/L sulfuric acid and 1g/L thiourea;
3. putting a platinum counter electrode into a hydrogen charging solution through a wire guide 7, and fixing the upper cover body 3 and the lower shell 2 by using a fastening screw 4;
4. the whole device is fixed on a sample table top of the TI-premier through a screw hole, a lead wire welded to a sample and a platinum counter electrode are connected to an electrochemical workstation, and the TI-premier sample cabin door is closed.
5. Opening an electrochemical workstation according to the current density preset in the experiment, starting a flow pump, feeding the hydrogen charging solution into the lower shell 2 through a liquid inlet 11 by the flow pump, discharging the hydrogen charging solution into an external solution collecting container from a liquid outlet 12, and continuously circulating the hydrogen charging solution in the lower shell 2;
6. the specimen test area was found under a TI-premier light microscope and the machine was adjusted to the appropriate height. The sample stage is moved to bring the probe into the needle test well 6 and the experimental operation is performed after the level of the hydrogen charged solution has stabilized.
FIG. 4 is a diagram of 2205 duplex stainless steel at 10mA/cm 2 Before and after charging, a is before charging, b is after charging for 1 hour, and c is after charging for 5 hours. Experiments can be continuously carried out on line through the device, and the longer the charging time is, the rougher the surface of the sample is. A rough surface will result in greater displacement and lower calculated hardness than a smooth surface.
In conclusion, the device has novel structural design and convenient use, and can perform in-situ hydrogen charging test on the hydrogen charging sample. The invention is suitable for the instruments using probes for measuring such as nano indentation, atomic force microscope and the like.

Claims (2)

1. The utility model provides an in situ hydrogen charging experimental apparatus, includes base (1), lower casing (2) and upper cover body (3), its characterized in that: the longitudinal section of the lower shell (2) is of a convex structure, the lower shell (2) is fixed on the base (1) through a locking bolt, symmetrically arranged through holes are formed in the lower shell (2) and the upper cover body (3), and the upper cover body (3) is fixed on the lower shell (2) through a fastening screw (4); the center of the lower shell (2) is provided with a cylindrical hollow inner cavity, the hollow inner cavity is provided with a carrying platform (5), and the height of the carrying platform (5) is lower than the upper edge of the hollow inner cavity; the center of the upper cover body (3) is provided with a needle head test hole (6), the needle head test hole (6) is arranged right above the carrier (5), the upper cover body (3) is also provided with a wire guide hole (7), a round sample welded with a wire is placed on the carrier (5), and the wire passes through the wire guide hole (7); protrusions (8) are arranged on two opposite sides of the upper protruding portion of the lower shell (2), and grooves (9) matched with the protrusions (8) are arranged on two opposite sides of the upper cover body (3); an outward overflow port (10) is formed in the boss (8); the side wall of the upper bulge of the lower shell (2) is provided with a liquid inlet (11), and the side wall of the opposite side is provided with a liquid outlet (12); a rubber sealing gasket is arranged at the joint between the lower shell (2) and the base (1);
the carrying platform (5) adopts a concave carrying platform, and the carrying platform (5) adopts a cylindrical structure;
the base (1), the lower shell (2) and the upper cover body (3) are all made of organic glass materials.
2. A method for performing an in situ hydrogen charging experiment using an in situ hydrogen charging experimental apparatus as defined in claim 1, wherein:
A. firstly, a liquid inlet (11) on a lower shell (2) is connected with a flow pump through a liquid inlet pipe, and a liquid outlet (12) is connected with a container through a liquid outlet pipe;
B. directly injecting the hydrogen charging solution into the lower shell (2) by using a syringe, so that the liquid level is 1 mm beyond the surface of the sample;
C. putting a platinum counter electrode into a hydrogen charging solution through a wire guide (7), and fixing an upper cover body (3) and a lower shell body (2) by using a fastening bolt;
D. connecting a lead and a platinum counter electrode welded on a sample to an electrochemical workstation, and opening the electrochemical workstation according to the current density preset in an experiment;
E. starting a flow pump, feeding the hydrogen charging solution into the lower shell (2) through a liquid inlet (11), discharging the hydrogen charging solution into an external container from a liquid outlet (12), and continuously circulating the hydrogen charging solution in the lower shell (2);
F. finally, after the liquid level of the hydrogen charging solution is stable, the operation probe enters the needle head test hole (6) for experimental operation.
CN201910555060.2A 2019-06-25 2019-06-25 In-situ hydrogen charging experimental device Active CN110133090B (en)

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Publication number Priority date Publication date Assignee Title
CN110954586B (en) * 2019-12-17 2022-04-26 武汉科技大学 In-situ hydrogen display detection device and detection method
CN113514513A (en) * 2021-07-13 2021-10-19 太原理工大学 Temperature-controllable in-situ electrochemical hydrogen charging and testing integrated device
CN113884410B (en) * 2021-09-13 2024-07-09 浙江大学 Device for observing hydrogen diffusion process of local tissue in material by using SKPFM
CN113884411B (en) * 2021-09-13 2024-07-09 浙江大学 Method for testing hydrogen diffusion coefficient of local tissue in material by using SKPFM

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WO2013187972A1 (en) * 2012-06-13 2013-12-19 Schmitz Roger William Environmental conditioning assembly for use in mechanical testing at micron or nano-scales
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KR20040051045A (en) * 2002-12-11 2004-06-18 (주)바이오니아 The hybridization device for biological sample
WO2013187972A1 (en) * 2012-06-13 2013-12-19 Schmitz Roger William Environmental conditioning assembly for use in mechanical testing at micron or nano-scales
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