CN108169263B - Grazing incidence experimental device for neutron small-angle scattering - Google Patents
Grazing incidence experimental device for neutron small-angle scattering Download PDFInfo
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- CN108169263B CN108169263B CN201810261529.7A CN201810261529A CN108169263B CN 108169263 B CN108169263 B CN 108169263B CN 201810261529 A CN201810261529 A CN 201810261529A CN 108169263 B CN108169263 B CN 108169263B
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- G01N23/202—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering using neutrons
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Abstract
The invention discloses a grazing incidence experimental device for neutron small-angle scattering. The experimental device comprises a collimation assembly, a fixed base, a depth scanning beam limiting assembly, a multi-dimensional motion assembly and a sample table assembly. The reflection experiment geometry adopted by the experimental device realizes the measurement of the thin film sample small-angle scattering signals, and the adopted beam limiting assembly with continuously adjustable beam limiting hole positions and sizes realizes the depth scanning of the large mechanical part surface layer small-angle scattering signals. The grazing incidence experimental device for small-angle neutron scattering is matched with a small-angle neutron scattering spectrometer, can effectively measure small-angle neutron scattering signals in a film sample and on the surface layer of a large mechanical part, can realize deep scanning of the structure of the large mechanical part near the surface layer, and has the characteristics of simple structure, reliable performance and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of environmental loading in neutron small-angle scattering application, and particularly relates to a grazing incidence experimental device for neutron small-angle scattering.
Background
Neutron small angle scattering is an effective means for nondestructive depth detection, can detect nano-to submicron-scale structural information in a solid or liquid system, and has important significance for material science, biopharmaceutical, physical research, engineering application and the like. The conventional small-angle experiment adopts transmission geometry, and the measurement signal is closely related to the thickness of the sample, so that the internal and mechanical part surface layer structural characteristics of the film sample are difficult to measure. The small angle scattering of the grazing incidence neutrons refers to small angle scattering signals generated when the neutrons are incident on the surface of the sample at a small angle, namely, at an angle near the critical angle of the material, and the reflection geometry is adopted, so that the nano-scale and submicron-scale structural information in the film sample and the structural change characteristics of the large mechanical parts in the depth direction can be measured.
The small angle neutron scattering technology is in a starting stage in China, and corresponding various technical developments are lacking. The Chinese patent literature library discloses a patent application named as vacuum cold and hot table for grazing incidence X-ray small angle scattering experiment (publication number: CN 106979957A), which provides a grazing incidence experiment measuring device suitable for X-ray small angle, but the collimation, shielding and integral structure of the invention are not suitable for neutron small angle scattering due to great difference between X-rays and neutrons.
Disclosure of Invention
The invention aims to provide a grazing incidence experimental device for neutron small-angle scattering.
The invention relates to a grazing incidence experimental device for neutron small-angle scattering, which is characterized by comprising a collimation assembly, a fixed base, a depth scanning beam limiting assembly, a multi-dimensional motion assembly and a sample platform assembly, wherein the collimation assembly is arranged on the fixed base;
the collimating assembly comprises a source diaphragm, a vacuum flying cavity and a sample diaphragm which are coaxial, wherein the vacuum flying cavity is a closed vacuum cavity which is horizontally arranged, the source diaphragm is arranged at the inlet end window, and the sample diaphragm is arranged at the outlet end window;
the depth scanning beam limiting assembly comprises an incident beam limiting device and an emergent beam limiting device; the upper surface of the fixed base is a plane, the upper surface is provided with a multi-dimensional motion assembly, the beam-in beam limiting device and the beam-out beam limiting device are symmetrically arranged on two sides of the multi-dimensional motion assembly, and the sample table assembly is fixed on the multi-dimensional motion assembly;
the multi-dimensional motion assembly comprises a three-dimensional translation device in the transverse direction, the longitudinal direction and the vertical direction and a three-dimensional rotation device around a transverse shaft, a longitudinal shaft and a vertical shaft; the sample table assembly comprises a sample fixing device and a composite shielding layer coated on the outer surface of the sample fixing device; the outer surfaces of the collimation component and the depth scanning beam limiting component are coated with neutron shielding materials;
the experimental device has the following working procedures:
neutron beams are incident from a source diaphragm, pass through a vacuum flight cavity, pass through a sample diaphragm, then are placed on the surface of a sample table assembly through an incident beam limiting device, are reflected or transmitted on the surface layer of the sample, and reach a neutron detector after passing through an emergent beam limiting device.
The inlet end window and the outlet end window of the vacuum flight cavity are made of sapphire or metal aluminum.
The vacuum flight cavity is provided with neutron conduits, and the number of the neutron conduits is adjustable.
The central positions and the sizes of the beam limiting holes of the beam limiting device for the incident beam and the beam limiting device for the emergent beam are continuously adjustable.
The described multi-dimensionsTranslational accuracy of the degree motion component is better than 0.1mm, and rotational accuracy is better than 0.05 o 。
The sample fixing device of the sample table assembly is a horizontal fixing device or a vertical fixing device.
The composite shielding layer of the sample table assembly comprises a neutron shielding layer and a gamma ray shielding layer.
The neutron shielding material is Cd, gd, 10 B、 6 One or more of Li.
The collimating component in the grazing incidence experimental device for neutron small angle scattering relies on a common neutron small angle scattering spectrometer, specific diaphragm sheets are added at the front end and the rear end, and the collimating distance is adjusted by adjusting the length of an accessed neutron catheter. The fixed base, the depth scanning beam limiting assembly, the multidimensional motion assembly and the sample table assembly are assembled into a whole, and the whole is placed at the sample table of the neutron small angle scattering spectrometer in the experimental process, so that the development of a conventional neutron small angle scattering experiment is not affected.
The grazing incidence experimental device for neutron small angle scattering improves the application range of neutron small angle scattering experiments by changing transmission optics into reflection optics, so that small angle neutron scattering signals in a film sample and on the surface layer of a large mechanical part can be effectively measured, and meanwhile, depth scanning of a structure of the large mechanical part near the surface layer can be realized, and the device has wide application prospect. The grazing incidence experimental device for neutron small-angle scattering has the characteristics of simple structure and reliable performance.
Drawings
FIG. 1 is a schematic diagram of the structure of a grazing incidence experimental setup for small angle neutron scattering of the present invention;
FIG. 2 is a top view of example 1 of the experimental setup for grazing incidence of neutron small angle scattering of the present invention;
FIG. 3 is a front view of example 1 of the experimental setup for grazing incidence of small angle scattering of neutrons of the present invention;
FIG. 4 is a left side view of example 1 of the experimental setup for grazing incidence of neutron small angle scattering of the present invention;
FIG. 5 is a front view of the multi-dimensional motion assembly of example 1 of the experimental setup for small angle scattering of neutrons of the present invention;
FIG. 6 is a top view of the sample stage assembly of example 1 of the experimental setup for small angle scattering of neutrons of the present invention;
FIG. 7 is a top view of the sample stage assembly of example 2 of the experimental setup for small angle scattering of neutrons of the present invention;
in the figure, neutron beam 11, source aperture 12, vacuum flight chamber 121, neutron tube 13, sample aperture 2, fixed base 31, incident beam limiting device 310, fixed bracket 311, horizontal beam limiting left blade 312, horizontal beam limiting right blade 313, vertical beam limiting upper blade 314, vertical beam limiting lower blade 32, beam limiting device 4, multi-dimensional motion assembly 41, transverse translation assembly 42, longitudinal translation assembly 43, vertical translation assembly 44, transverse axis rotation assembly 45, longitudinal axis rotation assembly 46, vertical axis rotation assembly 5, sample stage assembly 51, internal cavity 52, external composite shield 53, external vacuum hose 54, sample absorption aperture.
Detailed Description
The invention is described in detail below with reference to the drawings and examples.
The following 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, the grazing incidence experimental device for neutron small-angle scattering comprises a collimation component, a fixed base 2, a depth scanning beam limiting component, a multi-dimensional motion component 4 and a sample table component 5;
the collimation assembly comprises a source diaphragm 11, a vacuum flight cavity 12 and a sample diaphragm 13 which are coaxial, wherein the vacuum flight cavity 12 is a closed vacuum cavity which is horizontally arranged, the source diaphragm 11 is arranged at an inlet end window, and the sample diaphragm 13 is arranged at an outlet end window;
the depth scanning beam limiting assembly comprises an incident beam limiting device 31 and an emergent beam limiting device 32; the upper surface of the fixed base 2 is a plane, the upper surface is provided with a multi-dimensional motion assembly 4, an incident beam limiting device 31 and an emergent beam limiting device 32 are symmetrically arranged on two sides of the multi-dimensional motion assembly 4, and a sample table assembly 5 is fixed on the multi-dimensional motion assembly 4;
the multi-dimensional motion assembly 4 comprises a three-dimensional translation device in the transverse direction, the longitudinal direction and the vertical direction and a three-dimensional rotation device around a transverse axis, a longitudinal axis and a vertical axis; the sample table assembly 5 comprises a sample fixing device and a composite shielding layer coated on the outer surface of the sample fixing device; the outer surfaces of the collimation component and the depth scanning beam limiting component are coated with neutron shielding materials;
the experimental device has the following working procedures:
the neutron beam enters from the source diaphragm 11, passes through the vacuum flying cavity 12, passes through the sample diaphragm 13, enters the sample surface of the sample table assembly 5 through the input beam limiting device 31, is reflected or transmitted on the surface layer of the sample, and passes through the output beam limiting device 32 and reaches the neutron detector.
The inlet end window and the outlet end window of the vacuum flying cavity 12 are made of sapphire or metal aluminum.
The vacuum flying cavity 12 is provided with neutron tubes, and the number of the neutron tubes is adjustable.
The center positions and the sizes of the beam limiting holes of the input beam limiting device 31 and the output beam limiting device 32 are continuously adjustable.
The translational precision of the multidimensional motion component 4 is better than 0.1mm, and the rotational precision is better than 0.05 o 。
The sample fixing device of the sample table assembly 5 is a horizontal fixing device or a vertical fixing device.
The composite shielding layer of the sample table assembly 5 comprises a neutron shielding layer and a gamma ray shielding layer.
The neutron shielding material is Cd, gd, 10 B、 6 One or more of Li.
Example 1
As shown in fig. 2 to 6, in this embodiment, 0 is a neutron beam, the diameter of the source diaphragm 11 is 4 mm, the diameter of the sample diaphragm 13 is 2 mm, the length of the vacuum flight chamber 12 is 11 m, and the length of the neutron tube 121 is 2 m, so as to obtain the collimation distance 11-2=9 m.
In this embodiment, the beam limiting device 31 and the beam limiting device 32 are connected to the fixed base 2 through the fixed bracket 310, and each of the beam limiting device and the beam limiting device is composed of four-blade four-drive devices that move independently, including a horizontal beam limiting left blade 311, a horizontal beam limiting right blade 312, a vertical beam limiting upper blade 313 and a vertical beam limiting lower blade 314.
In this embodiment, the multi-dimensional motion stage assembly 4 includes a six-dimensional motion assembly, which is a horizontal translation assembly 41, a longitudinal translation assembly 42, a vertical translation assembly 43, a horizontal axis rotation assembly 44, a vertical axis rotation assembly 45, and a vertical axis rotation assembly 46 in this order from bottom to top.
In this embodiment, the sample stage assembly 5 is composed of an inner cavity 51 and an outer composite shielding layer 52, and the outer composite shielding layer 52 is composed of a 50mm thickness aluminum bracket, a 5mm thickness lead shielding layer and a 3mm thickness cadmium shielding layer from inside to outside in sequence. The internal cavity 51 is connected to a mechanical pump by an external vacuum hose 53 while being in communication with air through a sample adsorption port 54. When the sample is placed on the upper surface of the sample stage assembly 5, the mechanical pump is turned on, so that the sample is firmly adsorbed on the surface of the sample stage assembly 5.
In this embodiment, the lateral translation assembly 41, the longitudinal translation assembly 42, and the vertical translation assembly 43 ensure that the upper surface of the sample is aligned with the neutron beam 0 by moving the assembly 44 about the lateral axis and the assembly 45 about the longitudinal axis to ensure that the surface of the sample is parallel to the horizontal plane. During the experiment, the angle of incidence of the neutron beam 0 with the sample surface was controlled by the angle of rotation of the rotating assembly 45 about the longitudinal axis.
Example 2
The implementation of this example is substantially the same as example 1, except that the sample stage of this example is adapted to measure a sample with a surface perpendicular to the horizontal plane, and fig. 7 is a top view of the sample stage assembly 5. The bottom of the sample stage assembly 5 is fixed to the upper surface of the multi-dimensional motion assembly 4 and translates or rotates with it, and the magnitude of the incident angle of the incident neutron beam 0 to the sample surface is controlled by the angle of rotation of the rotation assembly 46 about the vertical axis.
Claims (7)
1. The grazing incidence experimental device for neutron small-angle scattering is characterized by comprising a collimation assembly, a fixed base (2), a depth scanning beam limiting assembly, a multi-dimensional motion assembly (4) and a sample table assembly (5);
the collimating assembly comprises a source diaphragm (11), a vacuum flight cavity (12) and a sample diaphragm (13) which are coaxial, wherein the vacuum flight cavity (12) is a closed vacuum cavity which is horizontally arranged, the source diaphragm (11) is arranged at an inlet end window, the sample diaphragm (13) is arranged at an outlet end window, neutron tubes are arranged in the vacuum flight cavity (12), and the number of the neutron tubes is adjustable;
the depth scanning beam limiting assembly comprises an incident beam limiting device (31) and an emergent beam limiting device (32), wherein the incident beam limiting device (31) and the emergent beam limiting device (32) are connected to a fixed base (2) through a fixed bracket (310), and the incident beam limiting device (31) and the emergent beam limiting device (32) comprise a horizontal beam limiting left-side knife blade (311), a horizontal beam limiting right-side knife blade (312), a vertical beam limiting upper-side knife blade (313) and a vertical beam limiting lower-side knife blade (314);
the upper surface of the fixed base (2) is a plane, the upper surface is provided with a multi-dimensional motion assembly (4), an incident beam limiting device (31) and an emergent beam limiting device (32) are symmetrically arranged on two sides of the multi-dimensional motion assembly (4), and the sample table assembly (5) is fixed on the multi-dimensional motion assembly (4); the multi-dimensional motion assembly (4) comprises a transverse translation assembly (41), a longitudinal translation assembly (42), a vertical translation assembly (43), a rotation assembly (44) around a transverse axis, a rotation assembly (45) around a longitudinal axis and a rotation assembly (46) around a vertical axis which are arranged from bottom to top;
the sample table assembly (5) comprises a sample fixing device and a composite shielding layer coated on the outer surface of the sample fixing device, wherein the composite shielding layer sequentially comprises a 50 mm-thick aluminum bracket, a 5 mm-thick lead shielding layer and a 3 mm-thick cadmium shielding layer from inside to outside; the sample fixing device is an internal cavity (51), the internal cavity (51) is connected with a mechanical pump through an external vacuum hose (53), and is communicated with air through a sample adsorption pore channel (54); the outer surfaces of the collimation component and the depth scanning beam limiting component are coated with neutron shielding materials.
2. The grazing incidence experimental setup for small angle scattering of neutrons according to claim 1, wherein: the inlet end window and the outlet end window of the vacuum flying cavity (12) are made of sapphire or metal aluminum.
3. The grazing incidence experimental setup for small angle scattering of neutrons according to claim 1, wherein: the center positions and the sizes of the beam limiting holes of the input beam limiting device (31) and the output beam limiting device (32) are continuously adjustable.
4. The grazing incidence experimental setup for small angle scattering of neutrons according to claim 1, wherein: the translational precision of the multi-dimensional motion assembly (4) is better than 0.1mm, and the rotational precision is better than 0.05 degrees.
5. The grazing incidence experimental setup for small angle scattering of neutrons according to claim 1, wherein: the sample fixing device of the sample table assembly (5) is a horizontal fixing device or a vertical fixing device.
6. The grazing incidence experimental setup for small angle scattering of neutrons according to claim 1, wherein: the composite shielding layer of the sample table assembly (5) comprises a neutron shielding layer and a gamma ray shielding layer.
7. The grazing incidence experimental setup for small angle scattering of neutrons according to claim 1, wherein: the neutron shielding material is Cd, gd, 10 B、 6 One or more of Li.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810261529.7A CN108169263B (en) | 2018-03-28 | 2018-03-28 | Grazing incidence experimental device for neutron small-angle scattering |
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| CN201810261529.7A CN108169263B (en) | 2018-03-28 | 2018-03-28 | Grazing incidence experimental device for neutron small-angle scattering |
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| CN108169263B true CN108169263B (en) | 2023-05-05 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110109173B (en) * | 2019-05-24 | 2020-09-25 | 东莞中子科学中心 | Neutron insert system capable of achieving rapid installation and remote adjustment |
| CN110146527A (en) * | 2019-07-01 | 2019-08-20 | 哈尔滨工业大学 | A kind of pitch three-dimensional microstructures based on small-angle neutron scattering technology determine method |
| CN110567997B (en) * | 2019-10-11 | 2024-07-12 | 中国科学院上海应用物理研究所 | Vacuum cavity assembly for scattering experiment station |
| CN113204110A (en) * | 2021-05-07 | 2021-08-03 | 中国原子能科学研究院 | Neutron bicrystal monochromator and monochromatic neutron detection system |
| CN114518376B (en) * | 2022-02-18 | 2024-08-23 | 中国核动力研究设计院 | Electron probe shielding sample seat for radioactive sample |
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