In-situ device and method for measuring curvature change of sample in ion irradiation process

Abstract

The invention discloses an in-situ device and method for measuring curvature change of a sample in an ion irradiation process, and the in-situ device comprises a sample clamping and beam measurement assembly which is used for positioning the sample in the irradiation direction of an ion beam, can achieve the safe clamping of the sample and the free generation of curvature change at the same time, and is used for measuring the curvature change of the sample. The measurement of irradiation fluence, temperature and curvature can be realized at the same time; the temperature measurement and control assembly can measure and control the temperature of the sample; the in-situ profile measurement assembly can realize in-situ surface curvature measurement of the sample in the irradiation and heating processes; the vacuum component is used for providing a vacuum environment for the components; and the in-situ device is arranged at the terminal of the ion accelerator to measure the curvature change of the sample in the ion irradiation process. The method can be used for researching material size change, modulus, thermal expansion rate change and the like caused by factors such as defects, crystal growth and helium bubbles in the irradiation process of materials, and provides means for research, development, screening and evaluation of nuclear materials.

Description

Technical Field

[0001] The present invention relates to the field of nuclear material irradiation assessment, and more specifically to an in-situ device and method for measuring the curvature change of a sample during ion irradiation. Background Art

[0002] Nuclear materials are irradiated by fast neutrons during their service. Due to the evolution of defects, the mechanical and thermal behaviors of the materials, such as size, modulus, and thermal expansion rate, will undergo significant changes. Testing these changing behaviors in material test reactors has the disadvantages of high cost, long cycle, and resource shortage. Therefore, a convenient and fast method is urgently needed to study these behaviors. Ion irradiation has great similarities with fast neutron irradiation and is often used to simulate fast neutron irradiation. However, the ion irradiation range is short, and special methods are needed to measure the changes in mechanical and thermal properties of the materials, such as size, modulus, and thermal expansion rate, after ion irradiation. It is a feasible method to use the curvature change of nuclear material sheets or fiber samples under ion irradiation conditions and combine model calculations to obtain the size and performance evolution behavior of nuclear materials. Summary of the invention

[0003] The purpose of the present invention is to provide an in-situ device and method for measuring the change of sample curvature during ion irradiation, so as to solve the problems of high cost, long cycle and shortage of resources in the prior art of testing the change behavior in the material test pile.

[0004] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0005] According to a first aspect of the present invention, there is provided an in-situ device for measuring the change in curvature of a sample during ion irradiation, the in-situ device comprising: a sample clamping and beam measurement assembly, for positioning the sample in the irradiation direction of the ion beam, so that the sample can be safely clamped while freely undergoing a change in curvature, and conveniently and simultaneously achieving the measurement of irradiation dose, temperature and curvature; a temperature measurement and control assembly, for achieving the measurement and control of the temperature of the sample; an in-situ profile measurement assembly, disposed behind the sample clamping and beam measurement assembly, for achieving the in-situ measurement of the surface curvature of the sample during irradiation and heating; and a vacuum assembly, comprising a vacuum chamber and a vacuum pump, for providing a vacuum environment for the temperature measurement and control assembly, the sample clamping and beam measurement assembly, and the in-situ profile measurement assembly; wherein the in-situ device is disposed at the terminal of an ion accelerator, for achieving the measurement of the change in curvature of the sample during ion irradiation.

[0006] Preferably, the temperature measurement and control component can achieve temperature control of the sample between -196°C and 1500°C.

[0007] Preferably, the temperature measurement and control assembly is electrically insulated from the sample holding and beam current measurement assembly to ensure accurate sample current measurement.

[0008] Preferably, the sample clamping and beam measurement assembly includes two metal sheets with a square hole in the middle. The two metal sheets can be combined together to clamp the sample between the two, so that part of the sample is exposed in the square hole in the middle of the metal sheets, so that the front side of the sample receives ion irradiation and the back side receives curvature measurement.

[0009] Preferably, the two metal sheets can be clamped together by screws or ceramic tubes.

[0010] Preferably, the in-situ profile measurement component uses a spectral confocal position sensor with a long focal length as a distance measurement element. The spectral confocal position sensor is installed on a scanning stage to achieve line scanning or surface scanning of the sample surface height, thereby obtaining the curvature of the sample.

[0011] Preferably, the in-situ profile measurement component has a measurement accuracy of better than 2 microns for the sample surface height.

[0012] Preferably, the in-situ profile measurement component is disposed on the back of the sample to avoid interfering with irradiation of the sample by the ion beam.

[0013] Preferably, the vacuum chamber is connected to a beam pipeline, and the temperature measurement and control component, the sample clamping and beam measurement component, and the in-situ profile measurement component are installed in the vacuum chamber.

[0014] Preferably, the temperature measurement and control component uses a water cooling element or a liquid nitrogen cooling copper sleeve to cool the sample.

[0015] According to a second aspect of the present invention, a method for measuring the change of sample curvature during ion irradiation is provided, comprising the following steps: S1: providing an in-situ device for measuring the change of sample curvature during ion irradiation as described above; S2: loading the sample into a sample clamping and beam measurement component, and realizing temperature measurement and control of the sample through a temperature measurement and control component; S3: providing an ion irradiated sample through an accelerator, and using an in-situ profile measurement component to measure the surface profile of the sample at regular intervals (typically 10 minutes) to obtain a relationship between the change of the sample curvature and the ion injection amount, and finally obtaining a relationship between the change of the sample size and the irradiation dose through calculation; heating the sample, measuring the profile of the sample every time the temperature rises by a certain temperature (typically 10°C), obtaining a relationship between the change of the sample curvature and the temperature, and finally obtaining a value of the thermal expansion coefficient of the sample after irradiation through calculation.

[0016] The main point of the invention is that it realizes for the first time the in-situ measurement of the curvature change of nuclear material samples during ion irradiation. By in-situ measuring the curvature change of nuclear material thin sheet samples, fiber samples, etc. during the ion irradiation process and the subsequent temperature change process, the changes in size, modulus and thermal conductivity of the nuclear material during the ion irradiation process are evaluated.

[0017] According to the present invention, the in-situ profile measurement component adopts a long-focal-length spectral confocal position sensor as a distance measurement element, and the sensor has a height measurement accuracy of better than 2 microns for the sample surface; the spectral confocal position sensor is installed on a scanning stage to realize line scanning or surface scanning of the sample surface height, and the scanning step length can be adjusted as needed; the surface profile of the sample is obtained by coupling the sample surface height and the sample surface position coordinates through the control system; and the sample curvature information is further obtained by fitting the surface profile.

[0018] According to the present invention, an in-situ device and method for measuring the curvature change of nuclear material samples during ion irradiation with high accuracy and excellent performance are provided. The in-situ device is arranged at the terminal of the ion accelerator, and is used to measure the curvature change of thin slice samples, fiber samples, etc. of nuclear materials during ion irradiation. The device measures the curvature change of the sample during irradiation and heating in situ through the in-situ profile measurement component, providing a means for studying the behavior of material size change, modulus and thermal expansion rate change caused by defects, crystal growth, helium bubbles and other factors during material irradiation, and providing a means for promoting the research and development, screening and evaluation of nuclear materials.

[0019] In summary, the device and method for in-situ measuring the curvature change of nuclear material samples during ion irradiation with precision and excellent performance provided by the present invention can realize convenient and quick in-situ measurement of the curvature change of materials under ion beam irradiation and high temperature environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 An in-situ device for measuring the curvature change of a sample during ion irradiation provided according to a preferred embodiment of the present invention is shown;

[0021] Figure 2 The sample holding and beam measurement components are shown. DETAILED DESCRIPTION

[0022] The present invention will be further described below in conjunction with specific examples. It should be understood that the following examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. Unless otherwise specified, the technical means used in the examples are conventional operations in the art, or according to the experimental methods recommended by the instrument and equipment manufacturers. The reagents and materials used in the examples can be obtained from commercial sources unless otherwise specified.

[0023] According to a preferred embodiment of the present invention, an in-situ device for measuring the curvature change of a sample during ion irradiation is provided, such as Figure 1 As shown, the in-situ device includes: a temperature measurement and control component 10, a sample clamping and beam measurement component 20, an in-situ profile measurement component 30, and a vacuum component 40.

[0024] Among them, the temperature measurement and control component 10 can realize the temperature measurement and control of the sample; the sample clamping and beam measurement component 20 is used to position the sample in the irradiation direction of the ion beam, which can realize the safe clamping of the sample while freely changing the curvature, and can conveniently realize the irradiation dose, temperature and curvature measurement at the same time; the in-situ profile measurement component 30 is arranged behind the sample clamping and beam measurement component 20, and can realize the in-situ surface curvature measurement of the sample during irradiation and heating; the vacuum component 40 includes a vacuum chamber 41 and a vacuum pump 42, the vacuum chamber 41 is connected to the beam pipe 60, and the temperature measurement and control component 10, the sample clamping and beam measurement component 20, and the in-situ profile measurement component 30 are all installed in the vacuum chamber 41; the in-situ device is arranged at the terminal of the ion accelerator to realize the measurement of the curvature change of the thin sheet or fibrous sample 50 during ion irradiation.

[0025] like Figure 2 As shown, the sample clamping and beam measurement assembly 20 includes two metal sheets 21 with a square hole in the middle. The two metal sheets can be combined together to clamp the sample 50 between the two, so that part of the sample is exposed in the square hole in the middle of the metal sheets, so that the front side of the sample receives ion irradiation and the back side receives curvature measurement.

[0026] The in-situ profile measurement component 30 uses a long focal length spectral confocal position sensor 31 as a distance measurement element. The spectral confocal position sensor 31 is installed on a scanning stage 32 to achieve line scanning or surface scanning of the sample surface height, thereby obtaining the curvature of the sample.

[0027] Example 1

[0028] In this embodiment, the detector in the in-situ contour measurement component adopts a vacuum-compatible spectral confocal position detector with a focal length of 75mm, and the scanning stage in the component adopts a piezoelectric ultrasonic motor to achieve rapid scanning of the sample surface profile. The metal in the sample clamping and beam measurement component is tantalum metal, and the window size left is 10×10mm; the sample tested is nuclear graphite material, and the sample is processed into a 3×5×0.04mm thin sheet, and the fixture clamps four samples at a time; the temperature measurement and control component uses a thermocouple placed in the sample clamping and beam measurement component accessories to measure and control the temperature, and an infrared imager is used to monitor the uniformity and stability of the sample temperature; the component uses a resistance wire wrapped around a ceramic tube to heat the sample to achieve uniform temperature control of the sample from room temperature to 1000°C; the component is equipped with a water cooling element to ensure that the temperature of the in-situ contour measurement component is not higher than 50°C. The in-situ contour measurement component, the sample clamping and beam measurement component, and the temperature measurement and control component are integrated in the vacuum component and placed at the terminal of the ion accelerator. A molecular pump and an oil-free mechanical pump are used to evacuate the vacuum to ensure that the vacuum is better than 10 -4 During the experiment, the accelerator provided 2MeV Ar with a flux of 1 microampere. + For ion irradiated samples, the surface profile of the sample is measured every half hour using an in-situ profile measurement component to obtain the relationship between the change in sample curvature and the ion injection rate. After calculation, the relationship between the change in sample size and the irradiation dose is finally obtained.

[0029] Example 2

[0030] In this embodiment, the in-situ profile measurement component uses a spectral confocal position detector with a focal length of 30mm; the metal in the sample clamping and beam measurement components is titanium, and the window size is 5×5mm; the sample tested is a gallium nitride film, the sample size is 3×5×0.02mm thin film, and the fixture clamps one sample at a time; the temperature measurement and control component uses a thermocouple placed in the sample clamping and beam measurement component accessories for temperature measurement and temperature control; the sample is cooled by a liquid nitrogen cooling copper sleeve to achieve temperature control of the sample from -196℃ to room temperature. During the experiment, the accelerator provides 1MeV He with a flow rate of 500 nanoamperes + The sample was irradiated with ions and the temperature of the sample was controlled at -150°C. The surface profile of the sample was measured every half an hour using an in-situ profile measurement component to obtain the relationship between the curvature of the sample and the ion injection amount. The ion injection amount reached 5×10 16 ion / cm 2 Afterwards, the sample was heated at a rate of 5°C / min, and the profile of the sample was measured every time the temperature increased by 10°C to obtain the relationship between the change of the sample curvature and the temperature. After calculation, the relationship between the change of the sample size and the irradiation dose and the thermal expansion coefficient of the sample after irradiation were finally obtained.

[0031] The above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. The above embodiments of the present invention can also be modified in various ways. All simple, equivalent changes and modifications made according to the claims and the description of the present invention fall within the scope of protection of the claims of the present invention. The contents not described in detail in the present invention are all conventional technical contents.

Claims

1. An in-situ device for measuring the curvature change of a sample during ion irradiation, characterized in that: The in-situ device comprises: The sample clamping and beam current measurement assembly is used to position the sample in the irradiation direction of the ion beam, which can realize the free change of curvature of the sample while safely clamping it, and can conveniently realize the measurement of irradiation injection, temperature and curvature at the same time; Temperature measurement and control components, which can measure and control the temperature of samples; An in-situ profile measurement component, disposed behind the sample clamping and beam measurement component, capable of realizing in-situ surface curvature measurement of the sample during irradiation and heating; and A vacuum component, comprising a vacuum chamber and a vacuum pump, for providing a vacuum environment for the temperature measurement and control component, the sample clamping and beam measurement component, and the in-situ profile measurement component; The in-situ device is arranged at the terminal of the ion accelerator to measure the curvature change of the thin sheet or fiber sample during the ion irradiation process.

2. The in-situ device according to claim 1, characterized in that: The sample clamping and beam measurement assembly includes two metal sheets with a square hole in the middle. The two metal sheets can be combined to clamp the sample between the two, so that part of the sample is exposed in the square hole in the middle of the metal sheets, so that the front side of the sample receives ion irradiation and the back side receives curvature measurement.

3. The in-situ device according to claim 1, characterized in that: The temperature measurement and control component can realize temperature control of the sample between -196°C and 1500°C.

4. The in-situ device according to claim 1, characterized in that: The temperature measurement and control assembly is electrically insulated from the sample clamping and beam current measurement assembly to ensure accurate sample current measurement.

5. The in-situ device according to claim 1, characterized in that: The in-situ profile measurement component uses a long focal length spectral confocal position sensor as a distance measurement element. The spectral confocal position sensor is installed on a scanning platform to achieve line scanning or surface scanning of the sample surface height, thereby obtaining the curvature of the sample.

6. The in-situ device according to claim 1, characterized in that: The in-situ profile measurement component has a measurement accuracy of better than 2 microns for the sample surface height.

7. The in-situ device according to claim 1, characterized in that: The in-situ profile measurement component is arranged on the back of the sample to avoid interfering with the irradiation of the sample by the ion beam.

8. The in-situ device according to claim 1, characterized in that: The vacuum chamber is connected to the beam pipeline, and the temperature measurement and control component, the sample clamping and beam measurement component, and the in-situ profile measurement component are installed in the vacuum chamber.

9. The in-situ device according to claim 1, characterized in that: The temperature measurement and control component uses a water cooling element or a liquid nitrogen cooling copper sleeve element to cool the sample.

10. A method for measuring the change in curvature of a sample during ion irradiation, characterized in that: The following steps are involved: S1: Provide an in-situ device for measuring the change in curvature of a sample during ion irradiation according to any one of claims 1 to 9; S2: Load the sample into the sample holding and beam current measurement assembly, and measure and control the temperature of the sample through the temperature measurement and control assembly; S3: The accelerator provides ion irradiation samples, and the in-situ profile measurement component is used to measure the surface profile of the sample at regular intervals to obtain the relationship between the sample curvature and the ion injection amount, and finally the relationship between the sample size and the irradiation dose is obtained through calculation; The sample is heated up, and the contour of the sample is measured every time the temperature rises by a certain amount to obtain the relationship between the curvature of the sample and the temperature. The thermal expansion coefficient value of the sample after irradiation is finally obtained through calculation.

Images