CN108490008B - Neutron small angle scattering loading device for researching hydrogen corrosion on metal surface - Google Patents
Neutron small angle scattering loading device for researching hydrogen corrosion on metal surface Download PDFInfo
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Abstract
The invention discloses a neutron small-angle scattering loading device for researching hydrogen corrosion on a metal surface. The device realizes the superposition of sheet samples by utilizing a plurality of sample clamps, and ensures the uniform loading of hydrogen while increasing the neutron small-angle scattering signal in the hydride; the size of a hydrogen loading cavity is optimized by utilizing a metal welding and metal gasket mode, the high-temperature and high-pressure loading of hydrogen is guaranteed, and the interference of the hydrogen on neutron small-angle scattering experiments is obviously reduced; the buffer tank matched with the hydrogen loading cavity and the pressure monitor play a role in maintaining experiments and feeding back hydrogen pressure. The device effectively acquires neutron small-angle scattering signals of hydrogen corrosion on the metal surface, and simultaneously solves the problems of hydrogen leakage at high temperature and high pressure and interference on experimental precision. The device combines neutron small angle scattering technology, can in-situ study the microstructure change of active metal in the hydrogen etching process, and makes up the defect of the conventional method in the early microstructure analysis of hydrogen etching.
Description
Technical Field
The invention belongs to the field of metal corrosion research, and particularly relates to a neutron small-angle scattering loading device for researching hydrogen corrosion on a metal surface.
Background
The industrial application of hydrogen to metal materials is remarkable, when the metal materials are stored for a long time in a small amount of hydrogen atmosphere, the high-activity metal is easy to generate surface corrosion, compared with oxidation corrosion, the hydrogenation corrosion reaction is more severe and is accompanied by remarkable volume expansion, and the product is inflammable, so that the mechanical property of the materials is easy to be reduced and the safety risk is easy to cause, and the metal materials are paid attention to the majority of researchers. The key process of metal hydrogenation corrosion is early hydride nucleation, and research on the evolution rule is a precondition for revealing the mechanism of hydrogenation corrosion and regulating corrosion resistance. However, the method is limited by analysis means, and the evolution rule of the hydride microstructure at the initial stage of the reaction is still not clear.
At present, a local analysis means is mainly adopted to observe the hydride on the metal surface. Wherein the high resolution optical microscope is suitable for observing the growth behavior of the hydride in the later stage of the reaction. The high-resolution scanning electron microscope and the electron back scattering technology have strict requirements on sample preparation, and the electron probe and the X-ray are insensitive to hydrogen elements and are easily influenced by oxides. Secondary ion mass spectrometers can obtain localized hydrogen distributions, but are destructive tests and cannot be dynamically observed. The resolution of an atom probe tomography microscope is high but no information on the structure of the hydride at a specific depth, especially in the presence of an oxide layer, is given. The analysis method is limited by the small penetration depth, low hydrogen sensitivity and harsh sample preparation conditions, and the analysis method is slow in the aspect of hydride dynamic observation at the initial stage of the interaction of metal and hydrogen.
The neutron small angle scattering can obtain the information of the size, distribution, content and the like of the nano-scale structure in the material, has the advantages of nondestructive detection, deep penetrability and the like, is very sensitive to hydrogen element, and has wide application prospect in the aspect of hydrogen corrosion analysis of the metal surface. The neutron small angle scattering technology is used for researching the hydride in the bulk metal internationally, but the effective signal is difficult to obtain experimentally because the hydride corroded by the surface hydrogen is few, so the neutron small angle scattering analysis of the surface hydrogen corrosion is not reported yet. In order to realize the neutron small angle scattering analysis of the hydrogen corrosion on the metal surface, the problems of effective observation of a small amount of hydride scattering signals on the surface and uniform loading of hydrogen are solved. Moreover, in terms of neutron small angle scattering experiments, the loading of hydrogen has its specificity: neutrons are very sensitive to hydrogen, and the hydrogen on a neutron optical path can interfere with the accuracy of an experimental result; many materials are easy to interact with hydrogen when being heated, so that a loading system is unstable; the hydrogen has high requirement on the tightness, and the common sealing mode at high temperature and high pressure is difficult to meet the requirement. The in-situ loading device for hydrogen corrosion on the metal surface is required to effectively acquire neutron small-angle scattering signals, and various problems in hydrogen loading are required to be comprehensively considered from the aspects of design, materials and process. The Chinese patent literature library discloses a patent (ZL 201510224536.6) named as a heat table for small-angle scattering experiments, which is a small-angle scattering in-situ heating device, is a general in-situ temperature loading device, and can not solve the signal acquisition problem of metal surface hydride, consider a series of problems faced by hydrogen loading and can not meet the neutron small-angle scattering experiment requirement of metal surface hydrogen corrosion although the device also has a gas loading function.
Disclosure of Invention
The invention aims to solve the technical problem of providing a neutron small-angle scattering loading device for researching hydrogen corrosion on the metal surface.
The invention relates to a neutron small angle scattering loading device for researching metal surface hydrogen corrosion, which is characterized by comprising a hydrogen loading cavity, a plurality of sample clamps arranged in the center of the hydrogen loading cavity, a cavity heating component arranged outside the hydrogen loading cavity, a buffer tank, a switching valve and an inflation system which are sequentially connected with the hydrogen loading cavity through a gas pipeline, wherein the buffer tank heating component is wrapped outside the buffer tank, and a pressure monitor monitors the internal pressure of the hydrogen loading cavity;
the hydrogen loading cavity is a tank-shaped container, the main body of the tank-shaped container is a rear end shell, a scattering window II is arranged at the bottom of the rear end shell, the cover body of the tank-shaped container is a front end shell, a scattering window I is arranged at the top of the front end shell, the outer diameters of the front end shell and the rear end shell are R1, a metal gasket is arranged between the front end shell and the rear end shell, the outer diameter of the metal gasket is R2, R1 is more than R2, fastening bolts are uniformly distributed in the circumferential direction between the R1 and the R2, and the fastening bolts are fixedly connected with the front end shell and the rear end shell; the front end shell, the rear end shell and the metal gasket are coaxial and have the same inner diameter;
the two ends of the sample clamp are annular supporting frames, the supporting rods are uniformly distributed on the annular supporting frames along the circumferential direction, a plurality of groups of gaskets are arranged on the supporting rods, and sheet samples are clamped between each group of gaskets.
The length of the inside of the hydrogen loading cavity along the neutron incidence direction is less than or equal to 1.5cm.
The volume of the hydrogen loading cavity is V1, the volume of the buffer tank is V2, and V2 is more than or equal to 10V1.
Gaps are reserved between the hydrogen loading cavity and the sample clamps to realize hydrogen circulation.
The diffusion window I is in sealing connection with the front end shell in a metal welding mode, and the diffusion window II is in sealing connection with the rear end shell in a metal welding mode.
The material of the scattering window I and the scattering window II is sapphire or quartz.
The cavity heating component and the cache tank heating component are synchronously temperature-controlled.
The inflation system has the functions of vacuumizing, inflating and deflating.
The size design of the sample clamp, the hydrogen loading cavity and the cavity heating component meets the neutron scattering light path requirement, and besides a scattering window, no device component exists in a scattering angle alpha.
The clamp formed by the gasket, the support rod and the annular support frame in the neutron small-angle scattering loading device for researching the hydrogen corrosion on the metal surface is used for clamping a sheet sample; the scattering window, the front end shell, the rear end shell and the metal gasket form a sealed hydrogen loading cavity with a gas pipeline; the hydrogen stored in the buffer tank ensures the continuous performance of the hydrogen charging experiment; the loading cavity heating component and the buffer tank heating component are respectively used for heating the hydrogen loading cavity and the buffer tank, and synchronous temperature control is realized; the pressure monitor is used for measuring the hydrogen pressure change in the experimental process; the inflation system is used for vacuumizing and inflating and deflating hydrogen in the experimental process.
According to the neutron small angle scattering loading device for researching the hydrogen corrosion on the metal surface, disclosed by the invention, the clamping and hydrogen loading of a plurality of sheet samples are realized by using the gasket, the support rod and the annular support frame, and the neutron small angle scattering signal is improved by superposing and increasing the metal surface area measured through experiments; compared with the sealing mode of adding water to circulate and cool (or other cooling liquid) a conventional rubber gasket, the metal welding and metal gasket sealing structure is simple, high-temperature and high-pressure resistant, occupies smaller volume and has no gas emission, the size of a hydrogen loading cavity is reduced to the greatest extent, and the interference of hydrogen on the neutron small-angle scattering experimental precision is obviously reduced; the buffer tank and the hydrogen loading cavity are synchronously temperature-controlled, so that the problem that the hydrogen content in the small-volume hydrogen loading cavity is insufficient to complete the experiment is solved. The device provided by the invention can be used for in-situ research on the microstructure change of active metal in the hydrogen etching process by combining a neutron small-angle scattering technology, and the defect of the conventional method in the aspect of early microstructure analysis of hydrogen etching is overcome.
The neutron small angle scattering loading device for researching the hydrogen corrosion on the metal surface can effectively acquire the neutron small angle scattering signal of the hydrogen corrosion on the metal surface, and simultaneously solve the problems of hydrogen leakage at high temperature and high pressure and interference on experimental precision.
Drawings
FIG. 1 is a schematic diagram of a neutron small angle scattering loading device for researching hydrogen corrosion on a metal surface;
FIG. 2 is a front view (neutron incidence direction) of a neutron small angle scattering loading device for researching hydrogen etching on a metal surface according to the invention;
FIG. 3 is a rear view (neutron exit direction) of a neutron small angle scattering loading device for researching hydrogen corrosion on a metal surface of the invention;
fig. 4 is a front view (neutron incidence direction) of a neutron small angle scattering carrier device for researching hydrogen etching on a metal surface according to the invention.
In the figure, 11, front end housing 12, rear end housing 13, diffuser window I14, metal washer 15, fastening bolt 16, diffuser window II 21, gasket 22, support bar 23, sheet sample 24, annular support bracket 3, buffer tank 41, cavity heating element 42, buffer tank heating element 5, pressure monitor 6, inflation system 7, gas line 8, and on-off valve.
Description: the neutron incidence direction refers to the direction in which neutrons are incident from the outside of the scattering window i toward the scattering window ii.
Detailed Description
The details of the invention and its embodiments are further described below with reference to the accompanying drawings and examples.
These examples are merely further illustrative of the present invention and should not be construed as limiting the scope of the invention. While not essential to the invention, it is to be understood that the invention may be practiced otherwise than as specifically described.
As shown in fig. 1-4, the neutron small angle scattering loading device for researching metal surface hydrogen corrosion of the invention comprises a hydrogen loading cavity, a plurality of sample clamps arranged in the center of the hydrogen loading cavity, a cavity heating part 41 arranged outside the hydrogen loading cavity, a buffer tank 3, a switching valve 8 and an inflation system 6 which are sequentially connected with the hydrogen loading cavity through a gas pipeline 7, wherein the buffer tank heating part 42 is wrapped outside the buffer tank 3, and a pressure monitor 5 monitors the internal pressure of the hydrogen loading cavity;
the hydrogen loading cavity is a tank-shaped container, the main body of the tank-shaped container is a rear end shell 12, a scattering window II 16 is arranged at the bottom of the rear end shell 12, the cover body of the tank-shaped container is a front end shell 11, a scattering window I13 is arranged at the top of the front end shell 11, the outer diameters of the front end shell 11 and the rear end shell 12 are R1, a metal gasket 14 is arranged between the front end shell 11 and the rear end shell 12, the outer diameter of the metal gasket 14 is R2, R1-R2 is more than 0, fastening bolts 15 are uniformly distributed in the circumferential direction between the R1 and the R2, and the fastening bolts 15 are fixedly connected with the front end shell 11 and the rear end shell 12; the front end shell 11, the rear end shell 12 and the metal gasket 14 are coaxial and have the same inner diameter;
the two ends of the sample clamp are annular supporting frames 24, supporting rods 22 are uniformly distributed on the annular supporting frames 24 along the circumferential direction, a plurality of groups of gaskets 21 are arranged on the supporting rods 22, and sheet samples 23 are clamped between each group of gaskets.
The length of the inside of the hydrogen loading cavity along the neutron incidence direction is less than or equal to 15mm.
The volume of the hydrogen loading cavity is V1, the volume of the buffer tank 3 is V2, and V2 is more than or equal to 10V1.
Gaps are reserved between the hydrogen loading cavity and the sample clamps to realize hydrogen circulation.
The diffusion window I13 is in sealing connection with the front end shell 11 in a metal welding mode, and the diffusion window II 16 is in sealing connection with the rear end shell 12 in a metal welding mode.
The material of the scattering window I13 and the scattering window II 16 is sapphire or quartz.
The cavity heating part 41 and the cache tank heating part 42 are synchronously temperature-controlled.
The inflation system 6 has the functions of vacuumizing, inflating and deflating.
Example 1
The neutron beam size used in the neutron small angle scattering experiment of this embodiment is 8mm, and the fluence rate is 2×10 5 cm - 2 .s -1 。
In the embodiment, the inner diameter of the front end shell 11 and the rear end shell 12 of the hydrogen loading cavity is 20mm, the outer diameter is 30mm, and the materials are made of hydrogen-resistant stainless steel materials; the diameter of the scattering window I13 and the diameter of the scattering window II 16 are 24mm, sapphire is selected as a material, and the sapphire is respectively connected with the front end shell 11 and the rear end shell 12 in a metal welding mode; the inner diameter of the metal gasket 14 is 20mm, the outer diameter is 25mm, and red copper is selected as a material; the total length of the interior of the hydrogen loading chamber along the direction of the neutron beam was 5mm and the volume was about 1.6ml.
The diameter of the annular supporting frame 24 of the multi-piece sample clamp in the embodiment is 19.9mm; the distance between the support bars 22 in the symmetrical position is 14.2mm; the diameter of the gasket 21 is 1mm, the thickness is 0.2mm, and the number is 11; the sheet samples 23 were 14mm in diameter, 0.2mm in thickness and 10 in number.
The inner diameter of the cavity heating part 41 in this embodiment is 31mm, the outer diameter is 50mm, and the total length along the neutron beam direction is 120mm; the hydrogen loading chamber was located at about 60mm in the middle of the chamber heating element.
The volume of the buffer tank 3 in the embodiment is 100ml; the hydrogen loading cavity, the buffer tank 3 and the pressure monitor 5 form a closed system by using the switch valve 8, and the pressure monitor 5 monitors the hydrogen pressure change. The cavity heating part 41 and the buffer tank heating part 42 in the embodiment are regulated and controlled by the same temperature controller, so that synchronous temperature control is realized.
The inflation system 6 in this embodiment is provided with components such as a vacuum pump and a hydrogen cylinder, and the like, and the entire system is evacuated and inflated with hydrogen.
After the implementation, when a neutron scattering experiment is carried out, the scattering signal of the hydride can be improved by 20 times, meanwhile, the scattering signal of the metal is obviously inhibited, compared with a common in-situ loading device (the total length of the inside of a loading cavity along the neutron beam direction is generally more than 100 mm), the interference signal generated by hydrogen in the experiment is reduced to 3.1%, the buffer tank has enough hydrogen to maintain the experiment to be continuously carried out, the problem of hydrogen leakage can not be generated when the experiment is loaded at high temperature and high pressure, and the selected material can not decompose and release gas when being heated so as to interfere the reaction of the metal and the hydrogen.
Example 2
The structure of this example is the same as that of example 1, except that quartz is used as the material of the scattering windows i 13 and ii 16; the total length of the interior of the hydrogen loading chamber along the direction of the neutron beam was 15mm and the volume was about 7.4ml.
After the implementation, when a neutron scattering experiment is carried out, the scattering signal of the hydride can be improved by 20 times, meanwhile, the scattering signal of the metal is obviously inhibited, compared with a common in-situ loading device (the total length of the inside of a loading cavity along the neutron beam direction is generally more than 100 mm), the interference signal generated by hydrogen in the experiment is reduced to 13.3%, the buffer tank has enough hydrogen to maintain the experiment to be continuously carried out, the problem of hydrogen leakage can not be generated when the experiment is loaded at high temperature and high pressure, and the selected material can not be decomposed to release gas during heating so as to interfere the reaction of the metal and the hydrogen.
Claims (6)
1. A neutron small angle scattering loading device for researching hydrogen corrosion on metal surface is characterized in that: the device comprises a hydrogen loading cavity, a plurality of sample clamps arranged in the center of the hydrogen loading cavity, a cavity heating component (41) arranged outside the hydrogen loading cavity, a buffer tank (3), a switching valve (8) and an inflation system (6) which are sequentially connected with the hydrogen loading cavity through a gas pipeline (7), wherein the buffer tank heating component (42) is wrapped outside the buffer tank (3), and a pressure monitor (5) monitors the pressure of the hydrogen loading cavity;
the hydrogen loading cavity is a tank-shaped container, the main body of the tank-shaped container is a rear end shell (12), a scattering window II (16) is arranged at the bottom of the rear end shell (12), the cover body of the tank-shaped container is a front end shell (11), a scattering window I (13) is arranged at the top of the front end shell (11), the outer diameters of the front end shell (11) and the rear end shell (12) are R1, a metal gasket (14) is arranged between the front end shell (11) and the rear end shell (12), the outer diameters of the metal gasket (14) are R2, R1> R2, fastening bolts (15) are uniformly distributed in the circumferential direction between the R1 and the R2, and the fastening bolts (15) are fixedly connected with the front end shell (11) and the rear end shell (12); the front end shell (11), the rear end shell (12) and the metal gasket (14) are coaxial and have the same inner diameter;
the two ends of the sample clamps are annular supporting frames (24), supporting rods (22) are uniformly distributed on the annular supporting frames (24) along the circumferential direction, a plurality of groups of gaskets (21) are arranged on the supporting rods (22), and sheet samples (23) are clamped between each group of gaskets;
the material of the scattering window I (13) and the scattering window II (16) is sapphire or quartz;
the cavity heating component (41) and the buffer tank heating component (42) are synchronously temperature-controlled.
2. The neutron small angle scattering loading device for researching metal surface hydrogen corrosion of claim 1, wherein the length of the hydrogen loading cavity along the neutron incidence direction is less than or equal to 15mm.
3. The neutron small angle scattering loading device for researching hydrogen corrosion on a metal surface according to claim 1, wherein: the volume of the hydrogen loading cavity is V1, and the volume of the buffer tank (3) is V2, wherein V2 is more than or equal to 10V1.
4. The neutron small angle scattering loading device for researching hydrogen corrosion on a metal surface according to claim 1, wherein: gaps are reserved between the hydrogen loading cavity and the sample clamps to realize hydrogen circulation.
5. The neutron small angle scattering loading device for researching hydrogen corrosion on a metal surface according to claim 1, wherein: the scattering window I (13) is in sealing connection with the front end shell (11) in a metal welding mode, and the scattering window II (16) is in sealing connection with the rear end shell (12) in a metal welding mode.
6. The neutron small angle scattering loading device for researching hydrogen corrosion on a metal surface according to claim 1, wherein: the inflation system (6) has the functions of vacuumizing, inflating and deflating.
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| CN104833687A (en) * | 2015-05-06 | 2015-08-12 | 中国工程物理研究院核物理与化学研究所 | Hot stage for small-angle scattering experiment |
| CN104849148A (en) * | 2015-05-21 | 2015-08-19 | 中国工程物理研究院核物理与化学研究所 | In situ pressure loading device for neutron small-angle scattering |
| CN106053235A (en) * | 2016-07-25 | 2016-10-26 | 中国矿业大学(北京) | Nanoscale compressing, shearing and twisting device and method for small-angle scattering study of coal and rock materials |
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| CN104833687A (en) * | 2015-05-06 | 2015-08-12 | 中国工程物理研究院核物理与化学研究所 | Hot stage for small-angle scattering experiment |
| CN104849148A (en) * | 2015-05-21 | 2015-08-19 | 中国工程物理研究院核物理与化学研究所 | In situ pressure loading device for neutron small-angle scattering |
| CN106053235A (en) * | 2016-07-25 | 2016-10-26 | 中国矿业大学(北京) | Nanoscale compressing, shearing and twisting device and method for small-angle scattering study of coal and rock materials |
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