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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upper cover
lower housing
hydrogen
lower shell
cover body
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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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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

一种原位充氢实验装置An in-situ hydrogen charging experimental device

技术领域Technical field

本发明涉及电化学实验技术领域,具体为一种原位充氢实验装置。The invention relates to the technical field of electrochemical experiments, specifically an in-situ hydrogen charging experimental device.

背景技术Background technique

氢对几乎所有金属都有氢致塑性损减和氢致断裂抗性降低的不利影响,这些现象一般统称为氢脆。而材料在制备、加工和使用中都可能有氢进入材料。所以,研究氢对材料的影响成为安全、经济地使用材料的关键。Hydrogen has the adverse effects of hydrogen-induced plasticity loss and hydrogen-induced fracture resistance reduction on almost all metals. These phenomena are generally referred to as hydrogen embrittlement. Hydrogen may enter the material during its preparation, processing and use. Therefore, studying the effects of hydrogen on materials has become key to using materials safely and economically.

为了研究氢对材料的影响,需要对含氢的试样进行力学测试。常用的充氢方法有水溶液电解充氢、熔盐电解充氢和气相充氢,其中水溶液电解充氢因为其安全性和易操作性应用最广泛。In order to study the effect of hydrogen on materials, mechanical testing of hydrogen-containing specimens is required. Commonly used hydrogen charging methods include aqueous solution electrolytic hydrogen charging, molten salt electrolytic hydrogen charging and gas phase hydrogen charging. Among them, aqueous solution electrolytic hydrogen charging is the most widely used because of its safety and ease of operation.

常规的力学实验如单轴拉伸实验等,能够反映宏观尺度上氢对材料的影响。但随着研究的深入,微观尺度上氢对材料的影响尤其是氢对金属材料不同相的影响越来越重要。对微观尺度的研究往往需要使用细小的探针来确定研究的区域,如纳米压痕仪等设备。Conventional mechanical experiments, such as uniaxial tensile experiments, can reflect the impact of hydrogen on materials at the macro scale. However, with the deepening of research, the impact of hydrogen on materials at the microscopic scale, especially the impact of hydrogen on different phases of metallic materials, is becoming more and more important. Research on the microscopic scale often requires the use of small probes to determine the area of study, such as nanoindentation equipment and other equipment.

传统的测试方法都是对充氢后的试样取出进行测试,充氢完成到测试开始的间隔中材料中的氢会结合成氢气溢出,影响实验结果准确性;另外,为保证测试时的氢浓度,常对试样进行长时间充氢,会对试样表面产生损伤,不利于下一步试验。而原位测试可以使测试部位始终保持较高的氢浓度,可以降低充氢时间,且不会有氢气溢出。所以,实现对试样充氢的同时连续在线进行测试对研究氢对材料的影响十分有益。The traditional testing method is to take out the sample after hydrogen charging for testing. In the interval between the completion of hydrogen charging and the start of the test, the hydrogen in the material will combine into hydrogen and overflow, affecting the accuracy of the experimental results; in addition, in order to ensure the hydrogen content during the test concentration, often charging the sample with hydrogen for a long time will cause damage to the surface of the sample, which is not conducive to the next test. In-situ testing can always maintain a high hydrogen concentration at the test site, reduce hydrogen charging time, and prevent hydrogen gas from overflowing. Therefore, it is very beneficial to conduct continuous online testing while charging the sample with hydrogen to study the impact of hydrogen on materials.

如上所述,如纳米压痕仪等探针类的设备可以实现对材料微观尺度的性能测试,但目前还没有使这类设备实现对试样充氢的同时连续在线进行测试的装置,不足以满足目前微观尺度上研究材料氢脆现象的要求。As mentioned above, probe-type equipment such as nanoindenters can test the performance of materials at a microscopic scale. However, there is currently no device that enables such equipment to continuously test online while charging the sample with hydrogen, which is not sufficient. It meets the current requirements for studying the hydrogen embrittlement phenomenon of materials on a microscopic scale.

发明内容Contents of the invention

本发明的目的在于提供一种原位充氢实验装置,实现了对试样充氢的同时连续在线进行测试,以解决上述背景技术中提出的问题。The object of the present invention is to provide an in-situ hydrogen charging experimental device, which can realize continuous online testing of samples while charging hydrogen, so as to solve the problems raised in the above background technology.

为实现上述目的,本发明提供如下技术方案:In order to achieve the above objects, the present invention provides the following technical solutions:

一种原位充氢实验装置, 包括底座、下壳体和上盖体,所述下壳体纵截面为“凸”字形结构,所述下壳体通过锁紧螺栓固定在底座上,所述下壳体和上盖体上设有对称设置的通孔,所述上盖体通过紧固螺钉固定在下壳体上;所述下壳体的中心设有圆柱形空心内腔,空心内腔设有载台,载台的高度低于空心内腔的上沿;所述上盖体中心设有针头测试孔,且所述针头测试孔设置在载台正上方,所述上盖体上还开有导线孔;所述下壳体上凸部分的相对两侧设有凸起,所述上盖体相对两侧设有与凸起相匹配的凹槽;所述凸起内部设有向外的溢流口;所述下壳体上凸的侧壁设有进液口,相对另一侧侧壁设有出液口,;所述下壳体与底座之间连接处安装有橡胶密封垫。An in-situ hydrogen charging experimental device includes a base, a lower shell and an upper cover. The lower shell has a "convex" longitudinal cross-section, and the lower shell is fixed on the base through locking bolts. The lower shell and the upper cover are provided with symmetrically arranged through holes, and the upper cover is fixed on the lower shell through fastening screws; the center of the lower shell is provided with a cylindrical hollow inner cavity, and the hollow inner cavity is provided with There is a carrier platform, and the height of the carrier platform is lower than the upper edge of the hollow inner cavity; a needle test hole is provided in the center of the upper cover body, and the needle test hole is set directly above the carrier platform, and the upper cover body is also provided with a needle test hole. There are wire holes; protrusions are provided on opposite sides of the upper convex part of the lower housing, and grooves matching the protrusions are provided on opposite sides of the upper cover; and an outward-facing protrusion is provided inside the protrusion. Overflow port; the convex side wall of the lower housing is provided with a liquid inlet, and the opposite side wall is provided with a liquid outlet; a rubber sealing gasket is installed at the connection between the lower housing and the base.

优选的,所述载台采用下凹载台,所述载台采用圆柱体结构。Preferably, the carrier adopts a concave carrier, and the carrier adopts a cylindrical structure.

优选的,所述底座、下壳体和上盖体均采用有机玻璃高分子材料制成。Preferably, the base, lower shell and upper cover are all made of organic glass polymer material.

一种原位充氢实验装置使用方法包括以下步骤:A method of using an in-situ hydrogen charging experimental device includes the following steps:

A、首先将下壳体上的进液口通过进液管连接流量泵,再将出液口通过出液管连接容器;A. First, connect the liquid inlet on the lower shell to the flow pump through the liquid inlet pipe, and then connect the liquid outlet to the container through the liquid outlet pipe;

B、将焊接导线后的圆形试样放置在载台上,导线通过导线孔,用注射器将充氢溶液直接注入下壳体,使液面没过试样表面1毫米;B. Place the round sample after welding the wires on the stage, pass the wires through the wire holes, and use a syringe to inject the hydrogen-filled solution directly into the lower case so that the liquid level is 1 mm below the surface of the sample;

C、将铂对电极穿过导线孔放入充氢溶液中,再将上盖体与下壳体用紧固螺栓固定;C. Put the platinum counter electrode through the wire hole into the hydrogen charging solution, and then fix the upper cover and lower shell with fastening bolts;

D、将焊接于试样的导线、铂对电极连接至电化学工作站,再按实验预设的电流密度打开电化学工作站;D. Connect the wire welded to the sample and the platinum counter electrode to the electrochemical workstation, and then turn on the electrochemical workstation according to the preset current density of the experiment;

E、开启流量泵,流量泵将充氢溶液通过进液口送入下壳体内部,并从出液口排出至外部容器中,下壳体内部的充氢溶液不断循环;E. Turn on the flow pump, which sends the hydrogen-charging solution into the lower housing through the liquid inlet and discharges it from the liquid outlet to the external container. The hydrogen-charging solution inside the lower housing continuously circulates;

F、最后在充氢溶液液面稳定后,操作探针进入针头测试孔进行实验操作。F. Finally, after the hydrogen-filled solution level is stable, operate the probe into the needle test hole to perform experimental operations.

本发明的有益效果是:The beneficial effects of the present invention are:

(1)本发明结构设计新颖,使用方便,能够连续对充氢试样进行原位力学性能测试。本发明适用于纳米压痕、原子力显微镜等使用探针测量的仪器。(1) The invention has a novel structural design, is easy to use, and can continuously conduct in-situ mechanical property testing of hydrogen-charged samples. The invention is suitable for instruments using probes for measurement such as nanoindentation and atomic force microscopes.

(2)本发明采用流量泵来更新充氢溶液,保证了容器里有新鲜的溶液,保证了充氢的浓度。(2) The present invention uses a flow pump to update the hydrogen charging solution, ensuring that there is fresh solution in the container and ensuring the concentration of hydrogen charging.

(3)本发明上盖体的设置对探针起到了限位作用,保护了探针上方传感器的安全。(3) The arrangement of the upper cover of the present invention plays a role in limiting the position of the probe and protects the safety of the sensor above the probe.

(4)本发明设计紧凑,即使是探针较短的机器也能够正常使用。(4) The invention has a compact design and can be used normally even with machines with short probes.

(5)本发明使用下凹的载台,既限制了圆形试样的自由度,也确保了试样的刚度,从而使实验能顺利进行。(5) The present invention uses a concave stage, which not only limits the degree of freedom of the circular sample, but also ensures the stiffness of the sample, so that the experiment can proceed smoothly.

(6)本发明底座、下壳体和上盖体均采用高分子材料制成,其具有优异的耐磨、耐腐蚀性能,不易损坏,使用寿命长。(6) The base, lower shell and upper cover of the present invention are all made of polymer materials, which have excellent wear resistance and corrosion resistance, are not easily damaged, and have a long service life.

附图说明Description of the drawings

图1为本发明结构示意图。Figure 1 is a schematic structural diagram of the present invention.

图2为本发明下壳体结构示意图。Figure 2 is a schematic structural diagram of the lower housing of the present invention.

图3为本发明上盖体结构示意图。Figure 3 is a schematic structural diagram of the upper cover body of the present invention.

其中,1底座、2下壳体、3上盖体、4紧固螺钉、5载台、6针头测试孔、7导线孔、8凸起、9凹槽、10溢流口、11进液口、12出液口。Among them, 1 base, 2 lower shell, 3 upper cover, 4 fastening screws, 5 stage, 6 needle test holes, 7 wire holes, 8 protrusions, 9 grooves, 10 overflow port, 11 liquid inlet , 12 liquid outlets.

图4为2205双相不锈钢充氢前后的光学显微照片,a充氢前,b充氢1小时,c充氢5小时。Figure 4 shows optical micrographs of 2205 duplex stainless steel before and after hydrogen charging, a before hydrogen charging, b hydrogen charging for 1 hour, and c hydrogen charging for 5 hours.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述。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.

一种原位充氢实验装置, 包括底座1、下壳体2和上盖体3,所述下壳体2纵截面为“凸”字形结构,所述下壳体2通过锁紧螺栓固定在底座1上,所述下壳体2和上盖体3上设有对称设置的通孔,所述上盖体3通过紧固螺钉4固定在下壳体上2,所述下壳体2的中心设有圆柱形空心内腔,空心内腔设有载台5,载台5的高度低于空心内腔的上沿;所述上盖体3中心设有压痕针头测试孔6,且所述压痕针头测试孔6设置在载台5正上方,所述上盖体3上还开有接导线孔7,所述下壳体2上凸部分的相对两侧设有凸起8,所述上盖体3相对两侧设有与凸起8相匹配的凹槽9,所述凸起8内部设有向外的溢流口10,所述下壳体2上凸的侧壁一侧设有进液口11,相对另一侧设有出液口12,所述进液口11通过进液管连接流量泵,所述出液口12通过出液管连接容器,本发明采用流量泵来更新充氢溶液,保证了容器里有新鲜的溶液。所述下壳体2与底座1之间连接处安装有橡胶密封垫。An in-situ hydrogen charging experimental device, including a base 1, a lower housing 2 and an upper cover 3. The lower housing 2 has a "convex" shaped structure in its longitudinal section, and is fixed on the lower housing 2 by locking bolts. On the base 1, the lower housing 2 and the upper cover 3 are provided with symmetrically arranged through holes. The upper cover 3 is fixed to the lower housing 2 through fastening screws 4. The center of the lower housing 2 A cylindrical hollow inner cavity is provided, and the hollow inner cavity is provided with a platform 5. The height of the platform 5 is lower than the upper edge of the hollow inner cavity; the upper cover 3 is provided with an indentation needle test hole 6 in the center, and the The indentation needle test hole 6 is arranged directly above the carrier 5. The upper cover 3 is also provided with a wire connection hole 7. The opposite sides of the upper convex part of the lower housing 2 are provided with protrusions 8. The upper cover 3 is provided with grooves 9 matching the protrusions 8 on opposite sides. The protrusions 8 are provided with an outward overflow opening 10 inside. The upper convex side wall of the lower housing 2 is provided with a groove 9 There is a liquid inlet 11, and a liquid outlet 12 is provided on the opposite side. The liquid inlet 11 is connected to a flow pump through a liquid inlet pipe, and the liquid outlet 12 is connected to a container through a liquid outlet pipe. The present invention uses a flow pump to Renew the hydrogen charging solution to ensure there is fresh solution in the container. A rubber sealing gasket is installed at the connection between the lower housing 2 and the base 1 .

本发明中,上盖体3的设置对探针起到了限位作用,保护了探针上方传感器的安全。In the present invention, the arrangement of the upper cover 3 plays a position-limiting role for the probe and protects the safety of the sensor above the probe.

本发明中,载台5采用下凹载台,低于空心内腔的上沿,所述载台5采用圆柱体结构。本发明使用下凹的载台,即限制了圆形试样的自由度,也确保了试样的刚度,从而是实验能顺利进行。In the present 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 cylindrical structure. The present invention uses a concave stage, which not only limits the degree of freedom of the circular sample, but also ensures the stiffness of the sample, so that the experiment can proceed smoothly.

本发明中,底座1、下壳体2和上盖体3均采用有机玻璃高分子材料制成,其具有优异的耐磨、耐腐蚀性能,不易损坏,使用寿命长。In the present invention, the base 1, the lower shell 2 and the upper cover 3 are all made of organic glass polymer materials, which have excellent wear resistance and corrosion resistance, are not easily damaged, and have a long service life.

本发明原位充氢实验装置的使用方法包括以下步骤:The method of using the in-situ hydrogenation experimental device of the present invention includes the following steps:

A、首先将下壳体2上的进液口11通过进液管连接流量泵,再将出液口12通过出液管连接容器;A. First, connect the liquid inlet 11 on the lower housing 2 to the flow pump through the liquid inlet pipe, and then connect the liquid outlet 12 to the container through the liquid outlet pipe;

B、将焊接导线后的圆形试样放置在载台5上,导线通过导线孔7,用注射器将充氢溶液直接注入下壳体2,使液面没过试样表面1毫米;B. Place the circular sample after welding the wires on the stage 5, pass the wires through the wire holes 7, and use a syringe to directly inject the hydrogen-filled solution into the lower housing 2 so that the liquid level is 1 mm below the surface of the sample;

C、将铂对电极穿过导线孔7放入充氢溶液中,再将上盖体3与下壳体2用紧固螺钉4固定;C. Put the platinum counter electrode through the wire hole 7 and put it into the hydrogen charging solution, and then fix the upper cover 3 and the lower case 2 with the fastening screws 4;

D、将焊接于试样的导线、铂对电极连接至电化学工作站,再按实验预设的电流密度打开电化学工作站;D. Connect the wire welded to the sample and the platinum counter electrode to the electrochemical workstation, and then turn on the electrochemical workstation according to the preset current density of the experiment;

E、开启流量泵,流量泵将充氢溶液通过进液口11送入下壳体2内部,并从出液口12排出至外部容器中,下壳体2内部的充氢溶液不断循环;E. Turn on the flow pump, which sends the hydrogen-charged solution into the interior of the lower housing 2 through the liquid inlet 11, and discharges it from the liquid outlet 12 to the external container. The hydrogen-charged solution inside the lower housing 2 is continuously circulated;

F、最后在充氢溶液液面稳定后,操作探针进入针头测试孔6进行实验操作。F. Finally, after the hydrogen-charging solution level is stable, operate the probe into the needle test hole 6 to perform experimental operations.

实施例1Example 1

以在Hysitron公司TI-premier纳米压痕仪中对2205双相不锈钢的原位充氢测试为例,其具体实施方式如下所述:Taking the in-situ hydrogen charging test of 2205 duplex stainless steel in Hysitron's TI-premier nanoindentation instrument as an example, the specific implementation is as follows:

1.将下壳体2上的进液口11通过进液管连接流量泵,再将出液口12通过出液管连接溶液收集容器;1. Connect the liquid inlet 11 on the lower housing 2 to the flow pump through the liquid inlet pipe, and then connect the liquid outlet 12 to the solution collection container through the liquid outlet pipe;

2.将打磨并抛光后焊接导线的2205双相不锈钢圆形试样放入载台5,导线穿过导线孔7,用注射器将充氢溶液直接注入下壳体2,使液面没过试样表面1毫米,本例中充氢溶液选用含0.5mol/L硫酸和1g/L硫脲的混合溶液;2. Place the 2205 duplex stainless steel round specimen with the ground and polished wires welded onto the stage 5, pass the wires through the wire holes 7, and use a syringe to directly inject the hydrogen-filled solution into the lower housing 2 so that the liquid level does not pass the test. The sample surface is 1 mm. In this example, the hydrogenation solution is a mixed solution containing 0.5mol/L sulfuric acid and 1g/L thiourea;

3.将铂对电极穿过导线孔7放入充氢溶液中,再将上盖体3与下壳体2用紧固螺钉4固定;3. Put the platinum counter electrode through the wire hole 7 and put it into the hydrogen charging solution, and then fix the upper cover 3 and the lower case 2 with the fastening screws 4;

4.将装置整体通过螺孔固定在TI-premier的样品台面上,将焊接于试样的导线、铂对电极连接至电化学工作站,关闭TI-premier样品舱门。4. Fix the entire device on the sample table of TI-premier through the screw holes, connect the wires welded to the sample and the platinum counter electrode to the electrochemical workstation, and close the TI-premier sample compartment door.

5.按实验预设的电流密度打开电化学工作站,开启流量泵,流量泵将充氢溶液通过进液口11送入下壳体2内部,并从出液口12排出至外部溶液收集容器中,下壳体2内部的充氢溶液不断循环;5. Open the electrochemical workstation according to the current density preset by the experiment, and turn on the flow pump. The flow pump will send the hydrogen-charged solution into the interior of the lower housing 2 through the liquid inlet 11, and discharge it from the liquid outlet 12 to the external solution collection container. , the hydrogen-filled solution inside the lower housing 2 circulates continuously;

6.在TI-premier光学显微镜下找到试样测试区域并调整机器到合适高度。移动样品台到使探针进入针头测试孔6,在充氢溶液液面稳定后进行实验操作。6. Find the sample testing area under the TI-premier optical microscope and adjust the machine to the appropriate height. Move the sample stage so that the probe enters the needle test hole 6, and conduct the experimental operation after the hydrogen-charged solution level is stable.

图4为2205双相不锈钢在10mA/cm2的电流密度下充氢,充氢前后的光学显微照片,a为充氢前,b为充氢1小时后,c为充氢5小时后。通过该装置可以连续在线进行实验,可以看出,充氢时间越长,试样的表面越粗糙。与光滑表面相比,粗糙表面将导致更大的位移和更低的计算硬度。Figure 4 shows the optical micrographs of 2205 duplex stainless steel before and after hydrogen charging at a current density of 10 mA/ cm2 . a is before hydrogen charging, b is after 1 hour of hydrogen charging, and c is after 5 hours of hydrogen charging. Through this device, experiments can be conducted continuously online. It can be seen that the longer the hydrogen charging time, the rougher the surface of the sample. Rough surfaces will result in larger displacements and lower calculated hardness compared to smooth surfaces.

综上所述,本发明结构设计新颖,使用方便,能够对充氢试样进行原位充氢测试。本发明适用于纳米压痕、原子力显微镜等使用探针测量的仪器。In summary, the present invention has a novel structural design, is easy to use, and can conduct in-situ hydrogen charging tests on hydrogen-charged samples. The invention is suitable for instruments using probes for measurement such as nanoindentation and atomic force microscopes.

Claims (2)

1.一种原位充氢实验装置, 包括底座(1)、下壳体(2)和上盖体(3),其特征在于:所述下壳体(2)纵截面为“凸”字形结构,所述下壳体(2)通过锁紧螺栓固定在底座(1)上,所述下壳体(2)和上盖体(3)上设有对称设置的通孔,所述上盖体(3)通过紧固螺钉(4)固定在下壳体(2)上;所述下壳体(2)的中心设有圆柱形空心内腔,空心内腔设有载台(5),载台(5)的高度低于空心内腔的上沿;所述上盖体(3)中心设有针头测试孔(6),且所述针头测试孔(6)设置在载台(5)正上方,所述上盖体(3)上还开有导线孔(7),将焊接导线后的圆形试样放置在载台(5)上,导线通过导线孔(7);所述下壳体(2)上凸部分的相对两侧设有凸起(8),所述上盖体(3)相对两侧设有与凸起(8)相匹配的凹槽(9);所述凸起(8)内部设有向外的溢流口(10);所述下壳体(2)上凸的侧壁设有进液口(11),相对另一侧侧壁设有出液口(12);所述下壳体(2)与底座(1)之间连接处安装有橡胶密封垫;1. An in-situ hydrogen charging experimental device, including a base (1), a lower housing (2) and an upper cover (3), characterized in that: the lower housing (2) has a "convex" longitudinal cross-section structure, the lower housing (2) is fixed on the base (1) through locking bolts, the lower housing (2) and the upper cover (3) are provided with symmetrically arranged through holes, and the upper cover The body (3) is fixed on the lower housing (2) through fastening screws (4); the center of the lower housing (2) is provided with a cylindrical hollow inner cavity, and the hollow inner cavity is provided with a loading platform (5), which carries The height of the platform (5) is lower than the upper edge of the hollow inner cavity; a needle test hole (6) is provided in the center of the upper cover body (3), and the needle test hole (6) is set in front of the carrier platform (5). Above, the upper cover (3) is also provided with a wire hole (7). The circular sample after welding the wire is placed on the stage (5), and the wire passes through the wire hole (7); the lower shell Protrusions (8) are provided on opposite sides of the upper convex part of the body (2), and grooves (9) matching the protrusions (8) are provided on opposite sides of the upper cover body (3); There is an outward overflow port (10) inside the lower housing (8); the convex side wall of the lower housing (2) is provided with a liquid inlet (11), and the opposite side wall is provided with a liquid outlet. (12); A rubber sealing gasket is installed at the connection between the lower housing (2) and the base (1); 所述载台(5)采用下凹载台,所述载台(5)采用圆柱体结构;The carrier (5) adopts a concave carrier, and the carrier (5) adopts a cylindrical structure; 所述底座(1)、下壳体(2)和上盖体(3)均采用有机玻璃材料制成。The base (1), lower housing (2) and upper cover (3) are all made of organic glass materials. 2.利用权利要求1所述的一种原位充氢实验装置进行原位充氢实验的方法,其特征在于:2. A method for carrying out in-situ hydrogenation experiments using an in-situ hydrogenation experiment device according to claim 1, which is characterized in that: A、首先将下壳体(2)上的进液口(11)通过进液管连接流量泵,再将出液口(12)通过出液管连接容器;A. First connect the liquid inlet (11) on the lower housing (2) to the flow pump through the liquid inlet pipe, and then connect the liquid outlet (12) to the container through the liquid outlet pipe; B、用注射器将充氢溶液直接注入下壳体(2),使液面没过试样表面1毫米;B. Use a syringe to directly inject the hydrogen-charging solution into the lower housing (2) so that the liquid level is 1 mm below the surface of the sample; C、将铂对电极穿过导线孔(7)放入充氢溶液中,再将上盖体(3)与下壳体(2)用紧固螺栓固定;C. Put the platinum counter electrode through the wire hole (7) into the hydrogen charging solution, and then secure the upper cover (3) and the lower shell (2) with fastening bolts; D、将焊接于试样的导线、铂对电极连接至电化学工作站,再按实验预设的电流密度打开电化学工作站;D. Connect the wire welded to the sample and the platinum counter electrode to the electrochemical workstation, and then turn on the electrochemical workstation according to the preset current density of the experiment; E、开启流量泵,流量泵将充氢溶液通过进液口(11)送入下壳体(2)内部,并从出液口(12)排出至外部容器中,下壳体(2)内部的充氢溶液不断循环;E. Turn on the flow pump. The flow pump will send the hydrogen-filled solution into the inside of the lower housing (2) through the liquid inlet (11), and discharge it from the liquid outlet (12) to the external container. Inside the lower housing (2) The hydrogen-charged solution is continuously circulated; F、最后在充氢溶液液面稳定后,操作探针进入针头测试孔(6)进行实验操作。F. Finally, after the hydrogen-filled solution level is stable, operate the probe into the needle test hole (6) to perform experimental operations.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
JP2015059785A (en) * 2013-09-18 2015-03-30 新日鐵住金株式会社 Electrochemical nanoindentation test apparatus and test method thereof
CN106501109A (en) * 2016-09-13 2017-03-15 北京理工大学 The in-situ nano impression test platform of energy storage material under a kind of electrochemical hot atmosphere
CN106769781A (en) * 2017-01-26 2017-05-31 武汉科技大学 A kind of device and application method for testing metal material hydrogen penetrating quality
CN210136203U (en) * 2019-06-25 2020-03-10 南京工业大学 In-situ hydrogen charging experimental device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
JP2015059785A (en) * 2013-09-18 2015-03-30 新日鐵住金株式会社 Electrochemical nanoindentation test apparatus and test method thereof
CN106501109A (en) * 2016-09-13 2017-03-15 北京理工大学 The in-situ nano impression test platform of energy storage material under a kind of electrochemical hot atmosphere
CN106769781A (en) * 2017-01-26 2017-05-31 武汉科技大学 A kind of device and application method for testing metal material hydrogen penetrating quality
CN210136203U (en) * 2019-06-25 2020-03-10 南京工业大学 In-situ hydrogen charging experimental device

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