CN-121994711-A - Material surface in-situ diagnosis rapid sampling device, diagnosis device and diagnosis method based on cascading partial vacuum structure

CN121994711ACN 121994711 ACN121994711 ACN 121994711ACN-121994711-A

Abstract

The invention discloses a material surface in-situ diagnosis rapid sampling device, a diagnosis device and a diagnosis method based on a cascading partial vacuum structure, and relates to the technical field of material surface in-situ diagnosis. The device comprises a sampling head assembly, a differential air extraction system, a laser ablation module, a spectrum acquisition module and a gas sampling module, wherein the sampling head assembly comprises a cavity structure which is formed by nesting two or more than two stages, the differential air extraction system comprises a plurality of air extraction units, the air extraction units are in one-to-one correspondence with the sealed cavities, the laser ablation module is used for transmitting laser beams to the surface of a material to be tested in the innermost sealed cavity through optical windows which are arranged on each layer of cavity and are coaxially aligned along the vertical direction by a laser device, the spectrum acquisition module is used for acquiring emission spectrum signals of plasmas through the optical windows, and the gas sampling module is communicated with the sealed cavity. According to the invention, the sampling head assembly is arranged on the surface of the material to form a local sealing structure, so that the surface of the material can be detected on site.

Inventors

YU YAOWEI
Zuo Yijie
SUN HAO
WANG TAO
XU XIONGWEI
FENG BO
YANG XIUQUAN
ZUO GUIZHONG
HU JIANSHENG

Assignees

中国科学院合肥物质科学研究院

Dates

Publication Date: 20260508
Application Date: 20260409

Claims (11)

1. The rapid sampling device for the in-situ diagnosis of the material surface based on the cascade partial vacuum structure is characterized by comprising a sampling head assembly, a differential air extraction system, a laser ablation module, a spectrum acquisition module and a gas sampling module; the sampling head assembly comprises two or more than two stages of cavity structures which are nested, wherein the cavity structures comprise a cavity and a sealing structural member; the differential air extraction system comprises a plurality of air extraction units, and the air extraction units are in one-to-one correspondence with the sealed cavities; The laser ablation module is used for emitting laser beams to the surface of the material to be tested in the innermost sealed cavity through optical windows which are arranged on each layer of cavity and are coaxially aligned along the vertical direction by a laser device so as to ablate the surface of the material to be tested and generate plasma; the spectrum acquisition module is used for acquiring an emission spectrum signal of the plasma through the optical window; the gas sampling module is communicated with the innermost sealed cavity and is used for collecting gaseous products released in or after the laser ablation process and conveying the gaseous products to the mass spectrum analysis device for detection.
2. The rapid sampling device for in-situ diagnostics of a material surface based on a cascading partial vacuum structure according to claim 1, wherein the sampling port of the gas sampling module is disposed in the innermost sealed cavity and is directed towards the laser ablation area; And a flow limiting structure is arranged between the innermost sealed cavity and the gas sampling module, the flow limiting structure is a flow limiting small hole or a flow limiting channel, the flow limiting structure is used for sampling gas and maintaining a high vacuum state in the innermost sealed cavity, and the conduction capacity of the flow limiting structure is matched with the pumping speed of the second air pumping unit.
3. The rapid sampling device for in-situ diagnosis of a material surface based on a cascade partial vacuum structure according to claim 2, wherein the aperture of the flow-limiting orifice is in a range from a micron level to a millimeter level.
4. The rapid material surface in-situ diagnosis sampling device based on the cascade partial vacuum structure, which is disclosed in claim 1, is characterized in that the sampling head component is a cavity structure which is arranged in a two-stage nested manner, the cavity structure which is arranged in the two-stage nested manner comprises an outer cavity structure and an inner cavity structure which is arranged in the outer cavity structure, wherein the outer cavity structure comprises an outer cavity and a first sealing structural member which is arranged at the bottom of the outer cavity, the first sealing structural member and the surface of a material to be tested form an outer sealing cavity, the inner cavity structure comprises an inner cavity and a second sealing structural member which is arranged at the bottom of the inner cavity, the second sealing structural member and the surface of the material to be tested form an inner sealing cavity, and the inner sealing cavity is positioned in the outer sealing cavity; The differential pumping system comprises a first pumping unit and a second pumping unit.
5. The rapid sampling device for in-situ diagnostics of a material surface based on a cascading partial vacuum structure of claim 1, wherein the cavities in the nested arrangement are arranged coaxially.
6. The rapid sampling device for in-situ diagnosis of a material surface based on a cascade partial vacuum structure according to claim 1, wherein the sealing structure is an elastic sealing ring, a flexible sealing gasket or a deformable sealing structure so as to adapt to the roughness or curvature of the material surface to be tested; The air extractor group is a turbo molecular pump, a compound molecular pump, a dry vacuum pump or a combination thereof.
7. The rapid sampling device for in-situ diagnosis of the material surface based on the cascade partial vacuum structure according to claim 1 is characterized by further comprising a pressure monitoring unit for monitoring the pressure and the pressure rise rate of the sealed cavity in real time, wherein when the pressure of the sealed cavity at the outer layer is reduced to a preset pressure threshold value and the pressure rise rate is not higher than the preset pressure rise rate threshold value, a corresponding air extractor unit is started to further extract air from the sealed cavity at the innermost layer so as to establish a high vacuum environment in the sealed cavity at the innermost layer.
8. The rapid in-situ diagnostics sampling device for a material surface based on a cascading partial vacuum structure according to any one of claims 1 to 7, further comprising a control unit for synchronously triggering the laser ablation module, the spectrum acquisition module and the gas sampling module to achieve time-dependent acquisition of laser ablation events and corresponding spectrum signals and mass spectrum signals.
9. The material surface in-situ diagnosis device based on the cascade partial vacuum structure is characterized by comprising the material surface in-situ diagnosis rapid sampling device based on the cascade partial vacuum structure, and further comprising a mass spectrometry device for detecting gaseous products related to hydrogen, deuterium or tritium isotopes.
10. The material surface in-situ diagnosis device based on the cascade partial vacuum structure according to claim 9, further comprising a movable platform, wherein the material surface in-situ diagnosis rapid sampling device based on the cascade partial vacuum structure is installed on the movable platform to realize in-situ scanning detection of a plurality of positions of a material surface to be detected.
11. A method of in situ diagnosing a material surface using a cascading partial vacuum structure based material surface in situ diagnostic apparatus as claimed in claim 9 or 10, comprising the steps of: S1, positioning and pressing a sampling head assembly on the surface of a material to be tested, so that an outer cavity and an inner cavity respectively form an outer sealing cavity and an inner sealing cavity through corresponding sealing structural members and the surface of the material to be tested; S2, starting a first air extractor group communicated with the outer sealed cavity, and pre-extracting air from the outer sealed cavity; S3, when the pressure of the outer sealing cavity is reduced to a preset pressure threshold value, starting a second air extractor group communicated with the inner sealing cavity, and further extracting air from the inner sealing cavity to establish a high vacuum environment in the inner sealing cavity, wherein the atmospheric pressure of the high vacuum environment is not higher than 10 -3 Pa; S4, emitting laser pulses to the surface of the material to be detected through a laser ablation module, generating plasma in the high vacuum environment and collecting emission spectrum signals of the plasma; S5, collecting gaseous products released in or after the laser ablation process through a gas sampling module, and conveying the gaseous products to a mass spectrum analysis device for analysis; And S6, analyzing the elemental composition and the hydrogen isotope retention characteristic of the surface of the material to be tested based on the time correlation result of the spectrum data and the mass spectrum data.

Description

Material surface in-situ diagnosis rapid sampling device, diagnosis device and diagnosis method based on cascading partial vacuum structure Technical Field The invention relates to the technical field of material surface in-situ diagnosis, in particular to a material surface in-situ diagnosis rapid sampling device, a diagnosis device and a diagnosis method based on a cascading partial vacuum structure. Background In nuclear fusion devices, aerospace equipment and large industrial equipment, key structural materials are usually in service in high-temperature, irradiation or complex atmosphere environments for a long time, and the surface element composition and gas retention behavior of the key structural materials have important significance for material performance evaluation and service safety. Conventional material surface analysis methods typically require removal and transfer of the part to be tested to a laboratory environment for detection using thermal desorption spectroscopy, ion beam analysis, or other characterization equipment. However, the off-line detection method is long in period, pollution is easily introduced or the surface state of the material is easily changed in the processes of disassembly, transportation and storage, and the surface characteristics of the material under the actual service condition are difficult to truly reflect. The laser-induced breakdown spectroscopy (Laser Induced Breakdown Spectroscopy, LIBS) is a spectroscopic technology capable of realizing rapid elemental analysis, has the advantages of no need of complex sample preparation, high detection speed, realization of field detection and the like, and therefore, is widely focused in the field of rapid detection of material surfaces. However, when laser ablation is directly performed on the surface of a material in a conventional atmospheric environment, a background signal generated by air breakdown is strong, and meanwhile, oxidation reaction is easy to occur on the surface of the material, so that the spectrum detection sensitivity is reduced. In addition, the diffusion speed of the gaseous product released in the laser ablation process in the atmosphere is high, and effective collection and analysis of the gaseous product are difficult, so that synchronous analysis of the material element composition detection and the gas release characteristic is difficult to realize simultaneously. To reduce the air background and improve the detection sensitivity, the prior art proposes to perform LIBS detection in a vacuum environment. However, existing vacuum LIBS systems typically require that the sample to be tested be entirely placed in a vacuum chamber, which is difficult to implement for large equipment internal structures or non-removable components, limiting the application of this technique to in situ detection in the field. In addition, in the partial vacuum detection scheme, the technical problems are that, on one hand, in order to establish a high vacuum environment in a partial area of the surface of a material, the partial cavity is usually required to be pumped through a differential pumping structure, but when the surface roughness of the material is high or the sealing condition is limited under the field condition, the partial sealing space is easy to generate gas leakage, so that the high vacuum environment is difficult to establish stably, and on the other hand, when the mass spectrum detection is required to be carried out on the gas released in the laser ablation process, the gas sampling process can generate disturbance on the partial vacuum environment, if the design of the sampling structure is unreasonable, the vacuum degree of the cavity is possibly reduced, so that the stability of the laser ablation and the spectrum detection is influenced. Therefore, it is necessary to propose a material surface diagnosis technical scheme capable of rapidly establishing a stable high-vacuum environment in a local area of a material surface under the condition that the whole device to be tested is not required to be vacuumized, and effectively sampling gaseous products generated by laser ablation while maintaining a high-vacuum state, so as to realize combined in-situ analysis of spectrum detection and gas mass spectrum detection. Disclosure of Invention The invention provides a material surface in-situ diagnosis rapid sampling device based on a cascade partial vacuum structure, which aims to solve the problems that a stable high-vacuum environment is difficult to build on the material surface under the condition of on-site detection, the partial vacuum state is easy to break in the gas sampling process, the element information and the gas release information of the material surface are difficult to synchronously acquire and the like in the prior art. Correspondingly, the invention also provides a material surface in-situ diagnosis device and a diagnosis method based on the cascade partial vacuum structure. The de