Sample temperature and humidity control experimental device of neutron reflection type spectrometer
By designing a coaxial incident and exit position misalignment in the neutron reflectometer and combining it with the delivery of thermal insulation and reaction media, the problem of uncontrolled temperature and humidity in neutron reflectometer experiments has been solved, improving the accuracy of experimental results, especially in the study of soft matter and biofilms.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- CHINA SPALLATION NEUTRON SOURCE SCI CENT
- Filing Date
- 2026-04-07
- Publication Date
- 2026-06-09
AI Technical Summary
Existing neutron reflection experimental setups lack effective temperature and humidity control, resulting in an uncontrolled sample environment that affects the accuracy of experimental results, especially in the measurement of reflectance of soft matter and biologically related sample films.
An experimental device for sample temperature and humidity control of a neutron reflectance spectrometer was designed. By setting the coaxial incident and exit positions to be misaligned relative to the sample, and combining the thermal insulation medium delivery mechanism and the reaction medium delivery mechanism, the neutron reflectance test in the sample chamber is ensured to be carried out in a constant temperature and humidity environment.
This method enables neutron reflection testing of samples under controlled temperature and humidity conditions, improving the accuracy of experimental results. It plays a particularly important role in the study of the interface structure of polymers and biofilms under high humidity conditions.
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Figure CN122171594A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of experimental apparatus for neutron reflectance spectrometers with adjustable temperature and humidity, specifically to an experimental apparatus for controlling the sample temperature and humidity of a neutron reflectance spectrometer. Background Technology
[0002] Neutron scattering is a mature and routine method for probing the structure of matter and analyzing molecules using neutron beams. It is applied across a wide range of scientific fields, including physics, chemistry, biology, geology, mineralogy, and energy and environmental sciences. Compared to X-ray technology, neutron scattering possesses unique isotope discrimination capabilities, providing an irreplaceable research approach for studying alloy systems, fuel cells, complex organic molecules, and biomacromolecules. Neutrons are uncharged and have extremely strong penetrating power, facilitating in-situ real-time measurements in the application environment of materials. This advantage makes it crucial in materials science, extreme condition physics, and geological research.
[0003] Neutron reflection, an important neutron scattering technique, offers nanoscale depth resolution and high transmittance, making it a crucial tool for characterizing deep-layer excess interfacial absorption or accumulation of water in polymer films, nanocomposites, and metal / resin bonded materials. Compared to X-ray reflection, neutron reflection is advantageous because it is sensitive to light elements such as hydrogen, carbon, nitrogen, and oxygen, which are major components of soft matter. Furthermore, neutron reflection can distinguish between isotopes of these elements. A simple substitution of hydrogen with deuterium can significantly alter the scattering length distribution (SLD) profile of hydrogen-rich films with minimal impact on their chemical properties. By performing a series of reflectance measurements on the same system using different deuterium-labeled molecular components, more accurate structures can be obtained. Neutron reflection can typically explore film thicknesses from 10 Å to 2000 Å, making it a preferred technique for many experiments studying soft materials, thin magnetic films, and multilayer structures.
[0004] In neutron reflection experiments, the ambient temperature and humidity of the sample play an important role. Previously, there was no sample temperature and humidity control device for neutron reflection experimental setups. A temperature and humidity controlled environment can accelerate the study of neutron reflection of samples. Summary of the Invention
[0005] This application aims to provide a sample temperature and humidity control experimental device for a neutron reflectance spectrometer. A neutron beam is incident at a preset angle from the incident position onto the sample, and after reflection from the sample, it exits from the exit position, allowing for neutron reflection testing of the sample using a neutron reflectance spectrometer. Furthermore, by circulating a thermal insulation medium within the thermally insulated space to maintain the sample cavity in a constant temperature and humidity environment, the accuracy of the experimental results can be improved.
[0006] This application provides an experimental apparatus for sample temperature and humidity control in a neutron reflectance spectrometer, comprising:
[0007] A sample carrier assembly includes a housing, an entrance window assembly, an exit window assembly, and a sample holder. The housing has an entrance port and an exit port on opposite sides. The entrance window assembly and the exit window assembly are detachably mounted on the entrance port and the exit port, respectively, to enclose a sample cavity with the housing. The sample holder is detachably mounted in the sample cavity and is used to fix the sample, with opposite sides of the sample facing the entrance window assembly and the exit window assembly, respectively. A thermal insulation space is also provided between the inner and outer walls of the housing, surrounding the sample cavity. The entrance window assembly has an entrance position, and the exit window assembly has an exit position. The entrance position and the exit position are coaxial and offset from the sample on the sample holder.
[0008] A thermal insulation medium conveying mechanism is connected to the thermal insulation space and is used to circulate and convey thermal insulation medium into the thermal insulation space.
[0009] A reaction medium delivery mechanism is connected to the sample chamber and is used to circulate a reaction medium with a preset temperature and humidity into the sample chamber.
[0010] In one embodiment, a temperature and humidity sensor is further included, which extends into the sample chamber and is used to detect the temperature and humidity of the reaction medium within the sample chamber.
[0011] In one embodiment,
[0012] The entrance window assembly includes an entrance window and a first cover plate. The entrance window is installed at the entrance port. The first cover plate is detachably installed on the side of the housing where the entrance port is located and presses against the entrance window. The entrance position is located on the first cover plate.
[0013] The exit window assembly includes an exit window and a second cover plate. The exit window is installed at the exit port, and the second cover plate is detachably installed on the side of the housing where the exit port is located, and presses the exit window against it. The exit position is located on the second cover plate.
[0014] The entrance window, the exit window, and the housing together define the sample cavity.
[0015] In one embodiment, the first cover plate has a first opening at the incident position, and the second cover plate has a second opening at the exit position.
[0016] In one embodiment, the thermal insulation medium conveying mechanism includes a thermal insulation medium input connector and a thermal insulation medium output connector. The housing is provided with a thermal insulation medium inlet and a thermal insulation medium outlet. Both the thermal insulation medium inlet and the thermal insulation medium outlet are connected to the thermal insulation space. The thermal insulation medium input connector is installed at the thermal insulation medium inlet, and the thermal insulation medium output connector is installed at the thermal insulation medium outlet. The thermal insulation medium input connector is used to input thermal insulation medium into the thermal insulation space, and the thermal insulation medium output connector is used to output the thermal insulation medium from the thermal insulation space.
[0017] In one embodiment, the reaction medium delivery mechanism includes a reaction medium input connector and a reaction medium output connector. The housing is provided with a reaction medium inlet and a reaction medium outlet, both of which are connected to the sample chamber. The reaction medium input connector is installed at the reaction medium inlet, and the reaction medium output connector is installed at the reaction medium outlet. The reaction medium input connector is used to input the reaction medium into the sample chamber, and the reaction medium output connector is used to output the reaction medium from the sample chamber.
[0018] In one embodiment, the sample carrier assembly further includes a thermal insulation layer that covers the outer surface of the housing.
[0019] In one embodiment, the housing includes an inner shell, an outer shell, a first sealing plate, and a second sealing plate. The inner shell is installed inside the outer shell and connected to it. A gap exists between the inner shell and the outer shell. The first sealing plate covers one side of the inner shell and the outer shell and one side of the gap. The second sealing plate covers the other side of the inner shell and the outer shell and the other side of the gap. The first sealing plate, the second sealing plate, and the gap enclose the heat-insulating space. The heat-insulating layer covers the outer surface of the outer shell. The inner cavity of the inner shell, together with the entrance window and the exit window, encloses the sample cavity.
[0020] In one embodiment, the outer side of the housing facing the sample is further provided with a collimation position, which is used to collimate the sample at the sample position.
[0021] In one embodiment, the sample holder includes a base and two clamps. The base is detachably mounted in the sample cavity, and the two clamps cooperate with the base to clamp the two sides of the sample respectively.
[0022] The sample temperature and humidity control experimental apparatus of the neutron reflectance spectrometer according to the above embodiment, due to the coaxial incident and exit positions being offset relative to the sample, allows the neutron beam to enter from the incident position at a preset incident angle and irradiate the sample. After being reflected by the sample, it exits from the exit position and is captured by the neutron reflectance spectrometer. The interface structure of the sample can be obtained through analysis for neutron reflection testing. Furthermore, the circulating insulation medium within the insulation space ensures that the sample inside the sample chamber is maintained under a controlled and uniform preset temperature and humidity environment for neutron reflection testing, ensuring the accuracy of the test results. Attached Figure Description
[0023] Figure 1 The three-dimensional experimental apparatus for sample temperature and humidity control of the neutron reflectance spectrometer provided in this application Figure 1 ;
[0024] Figure 2 Explosion of the sample temperature and humidity control experimental apparatus for the neutron reflectance spectrometer provided in this application Figure 1 ;
[0025] Figure 3 The three-dimensional experimental apparatus for sample temperature and humidity control of the neutron reflectance spectrometer provided in this application Figure 2 ;
[0026] Figure 4 Explosion of the sample temperature and humidity control experimental apparatus for the neutron reflectance spectrometer provided in this application Figure 2 ;
[0027] Figure 5 The three-dimensional shell provided in this application Figure 1 ;
[0028] Figure 6 The three-dimensional shell provided in this application Figure 2 ;
[0029] Figure 7 A perspective view of the sample holder provided in this application.
[0030] Figure label:
[0031] Sample carrier assembly 10, housing 11, inner shell 111, inlet 1111, outlet 1112, outer shell 112, first sealing plate 113, second sealing plate 114, insulation medium inlet 115, insulation medium outlet 116, reaction medium inlet 117, reaction medium outlet 118, mounting hole 119, inlet window assembly 12, inlet window 121, first cover plate 122, first opening 123, outlet window assembly 13, outlet window 131, second cover plate 132, second opening 133, sample holder 14, seat body 141, clearance hole 1411, clamping plate 142, sample chamber 15, slot 151, insulation space 16, collimation position 17, bracket 18;
[0032] Insulation medium conveying mechanism 20, insulation medium input connector 21, insulation medium output connector 22;
[0033] Reaction medium conveying mechanism 30, reaction medium input connector 31, reaction medium output connector 32;
[0034] Temperature and humidity sensor 40;
[0035] Sample 100. Detailed Implementation
[0036] The present application will now be described in further detail with reference to the accompanying drawings and specific embodiments. Similar elements in different embodiments are referred to by related similar element reference numerals. In the following embodiments, many details are described to facilitate a better understanding of the present application. However, those skilled in the art will readily recognize that some features may be omitted in different situations, or may be replaced by other elements, materials, or methods. In some cases, certain operations related to the present application are not shown or described in the specification. This is to avoid obscuring the core parts of the present application with excessive description. For those skilled in the art, detailed description of these related operations is not necessary; they can fully understand the related operations based on the description in the specification and general technical knowledge in the art.
[0037] Furthermore, the features, operations, or characteristics described in the specification can be combined in any suitable manner to form various embodiments, and the operational steps involved in each embodiment can also be rearranged or adjusted in a manner that is obvious to those skilled in the art. Therefore, the specification and drawings are only for clearly describing a particular embodiment and do not imply that they represent the necessary components and / or order.
[0038] The serial numbers assigned to components in this document, such as "first" and "second," are used only to distinguish the described objects and have no sequential or technical meaning. The terms "connection" and "linkage" used in this application, unless otherwise specified, include both direct and indirect connections (linkages).
[0039] In related technologies, for the reflectance measurement of soft materials, especially biological membranes and polymer membranes (such as polyvinyl alcohol films and adhesives), precise control of the temperature and humidity of the sample environment is crucial. Water regions at material interfaces are evacuated in a dry state. In-situ observation of the interface structure under high humidity conditions is one of the most effective methods for elucidating the mechanisms of interfacial transition absorption and moisture accumulation. Controlled temperature and humidity environments can also accelerate the study of neutron reflectance in other industrially important functional polymers (such as polyelectrolyte membranes in fuel cells). The slow equilibration rate makes in-situ testing of polyelectrolyte membranes under humid conditions challenging.
[0040] To address the aforementioned issues, this application provides a sample temperature and humidity control experimental device for a neutron reflectance spectrometer. A neutron beam is incident at a preset angle from the incident position onto the sample, and after reflection from the sample, it exits from the exit position, allowing for neutron reflection testing of the sample using a neutron reflectance spectrometer. Furthermore, by circulating a thermal insulation medium within the thermal insulation space to maintain the sample cavity at a constant temperature and humidity, the accuracy of the experimental results can be improved.
[0041] See Figures 1-7 As shown, the sample temperature and humidity control experimental device for the neutron reflectance spectrometer provided in this embodiment includes a sample carrier assembly 10, a thermal insulation medium conveying mechanism 20, and a reaction medium conveying mechanism 30.
[0042] The sample carrier assembly 10 includes a housing 11, an entrance window assembly 12, an exit window assembly 13, and a sample holder 14. The housing 11 has an entrance port 1111 and an exit port 1112 on opposite sides, respectively. The entrance port 1111 and the exit port 1112 are set relative to the direction of neutron beam incident and exit. The entrance window assembly 12 is detachably mounted on the entrance port 1111, and the exit window assembly 13 is detachably mounted on the exit port 1112, forming a sample cavity 15 with the housing 11. The sample holder 14 is detachably mounted on the sample cavity 15. The sample holder 14 is used to fix the sample 100, and the opposite sides of the sample 100 face the entrance window assembly 12 and the exit window assembly 13, respectively.
[0043] It should be noted that the entrance window assembly 12 and the exit window assembly 13 are detachably installed in the entrance port 1111 and the exit port 1112, respectively. The sample holder 14 can be removed from the sample chamber 15 when the entrance window assembly 12 or the exit window assembly 13 is removed to replace the sample 100.
[0044] Since this application performs neutron reflection detection on sample 100, and sample 100 is film-shaped, the neutron beam needs to be incident at a preset incident angle (0.2°-5°) and pass through the incident window assembly 12 before irradiating sample 100. According to the principle of neutron reflectivity measurement, the neutron beam undergoes specular reflection on the surface of sample 100, with the reflection angle being the same as the incident angle. The neutron beam reflected from sample 100 passes through the exit window assembly 13 and leaves the sample cavity 15. To this end, the opposite sides of sample 100, fixed on sample holder 14, are positioned facing the incident window assembly 12 and the exit window assembly 13, respectively. The opposite sides of the film-shaped sample 100 are its opposite sides in the radial direction, and the incident neutron beam irradiates the surface of sample 100.
[0045] In this embodiment, to ensure the incident and exit positions of the neutron beam, an incident position is provided in the incident window assembly 12, and an exit position is provided in the exit window assembly 13. The incident position is the position where the neutron beam is perpendicularly incident, and the exit position is the position where the neutron beam irradiating the sample 100 exits after reflection. Since the incident angle and exit angle of the neutron beam are the same, the incident position and the exit position are coaxial. Furthermore, the coaxial incident position and exit position are misaligned with the sample 100 on the sample holder 14 to ensure that the neutron beam can enter from the incident position at a preset incident angle and exit from the exit position at the same reflection angle as the preset incident angle.
[0046] In one embodiment, the sample 100, fixed on the sample holder 14, is located at the center of the sample cavity 15. Alternatively, the center of the sample 100 can be considered to coincide with the center of the sample cavity 15. Based on the incident and exit angles of the neutron beam, the coaxial incident and exit positions are offset by 8 mm relative to the sample 100, precisely matching the incident and exit paths of the neutron beam. This ensures that the incident and reflected neutron beams can pass completely through the incident window assembly 12 and the exit window assembly 13 without offset or obstruction. The neutron beam reflected by the exit window assembly 13 is captured by the neutron reflection spectrometer detector. By analyzing the neutron reflection intensity distribution at different incident angles and based on neutron scattering theory, the interface structure of the sample (such as thickness, scattering length, density, etc.) can be determined.
[0047] In this embodiment, a heat-insulating space 16 is provided between the inner and outer walls of the shell 11, and the heat-insulating space 16 surrounds the sample cavity 15.
[0048] The insulation medium conveying mechanism 20 is connected to the insulation space 16. The insulation medium conveying mechanism 20 is used to circulate the insulation medium to the insulation space 16. The insulation medium can be water, oil or oil-water mixture at a preset temperature. Since the insulation space 16 is arranged around the sample cavity 15, the insulation medium at the preset temperature can circulate around the sample cavity 15, thereby keeping the sample cavity 15 warm.
[0049] The reaction medium delivery mechanism 30 is connected to the sample chamber 15. The reaction medium delivery mechanism 30 is used to circulate the reaction medium at a preset temperature and humidity (e.g., temperature of 80°C and relative humidity of 80%) to the sample chamber 15. The sample chamber 15 can ensure that the reaction medium inside it always maintains the preset temperature and humidity through the heat preservation medium in the heat preservation space 16, providing a uniform temperature and humidity environment for the sample 100. The reaction medium is usually a gas.
[0050] In this application, a support 18 is also connected to the bottom of the housing 11. The support 18 is used to connect to a moving mechanism. The moving mechanism can drive the housing 11 to move in three-dimensional space through the support 18 to align the incident position of the incident window assembly 12 with the neutron beam. The moving mechanism can be a sample stage in the spectrometer scattering chamber.
[0051] In the initial stage of the neutron reflection detection experiment, the entrance window assembly 12 or the exit window assembly 13 is removed, the sample holder 14 is disassembled and removed from the sample cavity 15, the sample 100 is fixed on the sample holder 14, the sample holder 14 with the sample 100 fixed is installed into the sample cavity 15, and the entrance window assembly 12 or the exit window assembly 13 is sealed. The insulation medium delivery mechanism 20 circulates the insulation medium to the insulation space 16, which can preheat the sample cavity 15 and prevent the reaction medium with the preset temperature and humidity from condensing due to excessively low temperature in the sample cavity 15. Subsequently, the reaction medium delivery mechanism 30 circulates a reaction medium at a preset temperature and humidity to the sample cavity 15. Once the sample cavity 15 is filled with the reaction medium, a neutron beam enters from the incident position of the incident window assembly 12 at a preset incident angle and irradiates the surface of the sample 100. After reflection from the surface of the sample 100, the neutron beam exits from the exit position of the exit window assembly 13. The exited neutron beam is captured by the neutron reflection spectrometer detector. By analyzing the neutron reflection intensity distribution at different incident angles and based on neutron scattering theory, the interface structure of the sample 100 (such as thickness, scattering length, density, etc.) can be determined, thus completing the neutron reflection detection of the sample 100. Afterward, the neutron beam generator is turned off, and the insulation medium delivery mechanism 20 and the reaction medium delivery mechanism 30 are also turned off. The above operation is repeated to test the next sample 100.
[0052] Because the coaxial incident and exit positions are offset relative to the sample, the neutron beam can enter from the incident position at a preset incident angle and irradiate the sample 100. After being reflected by the sample 100, it exits from the exit position and is then captured by a neutron reflectance spectrometer, allowing the interface structure of the sample 100 to be analyzed. Meanwhile, a circulating insulating medium within the thermal insulation space 16 ensures that the sample 100 within the sample chamber 15 is maintained in a controlled and uniform preset temperature and humidity environment for neutron reflectance testing, ensuring the accuracy of the test results.
[0053] See Figures 1-4 As shown, the entrance window assembly 12 includes an entrance window 121 and a first cover plate 122. The entrance window 121 is installed at the entrance port 1111. The first cover plate 122 is detachably installed on the side of the housing 11 where the entrance port 1111 is located, and presses the entrance window 121 to position the entrance window 121 at the entrance port 1111 by pressing the entrance window 121 with the first cover plate 122. The entrance position is located on the first cover plate 122. The exit window assembly 13 includes an exit window 131 and a second cover plate 132. The exit window 131 is installed at the exit port 1112. The second cover plate 132 is detachably installed on the side of the housing 11 where the exit port 1112 is located, and presses the exit window 131 to position the exit window 131 at the exit port 1112 by pressing the exit window 131 with the second cover plate 132. The exit position is located on the second cover plate 132. The incident window 121, the exit window 131, and the housing 11 together define the sample chamber 15.
[0054] In this embodiment, the first cover plate 122 has a first opening 123 at the entrance position, and the second cover plate 132 has a second opening 133 at the exit position. Both the entrance window 121 and the exit window 131 are circular aluminum windows (diameter: 96mm, thickness: 4mm) made of aluminum or aluminum alloy. Their shape and size are determined according to the shape and size of the entrance port 1111 and the exit port 1112. Aluminum has a low neutron absorption rate, which meets the requirement of high neutron beam transmittance. Furthermore, aluminum also has high temperature resistance and corrosion resistance, meeting the long-term use requirements of the entrance window 121 and the exit window 131 in high temperature and high humidity environments. The first opening 123 on the first cover plate 122 and the second opening 133 on the second cover plate 132 can be used for neutron beam incident and exit respectively. The dimensions of the first opening 123 and the second opening 133 (length: 10mm, width: 42mm) are determined according to the size of the neutron beam spot to ensure that the neutron beam can be completely incident from the first opening 123 at a preset angle and irradiate the surface of the sample 100, and accurately exit from the second opening 133 of the exit window 131 after reflection.
[0055] See Figure 5 As shown, to ensure the collimation of the neutron beam, a collimation position 17 is provided on the outer side of the housing 11 facing the sample 100. The collimation position 17 is used to collimate the sample 100 on the sample holder. The collimation position 17 is aligned with the center of the sample 100. The collimation position 17 can be a crosshair. The collimation of the sample 100 can be completed by irradiating the crosshair intersection of the collimation position 17 with a laser perpendicularly.
[0056] The sample temperature and humidity control experimental apparatus for the neutron reflectometer provided in this application further includes a temperature and humidity sensor 40, which extends into the sample chamber 15 and is used to detect the temperature and humidity of the reaction medium within the sample chamber 15. A mounting hole 119 is provided on the housing 11, which extends through into the sample chamber 15. The temperature and humidity sensor 40 is installed in the mounting hole 119, and its detection end extends into the sample chamber 15 to accurately obtain the temperature and humidity of the reaction medium within the sample chamber 15.
[0057] Of course, the detection end of the temperature and humidity sensor 40, which extends into the sample chamber 15, should be close to the sample 100 to improve measurement accuracy.
[0058] The reaction medium with preset temperature and humidity can be quantitatively generated by a temperature and humidity generator. This quantitatively generated reaction medium with preset temperature and humidity can be transported to the sample chamber 15 via a reaction medium transport mechanism 30. During transport, the gas inside the sample chamber 15 can be displaced, gradually filling the sample chamber 15. The temperature and humidity sensor 40 can be electrically connected to the temperature and humidity generator. The temperature and humidity sensor 40 feeds back the detected temperature and humidity information inside the sample chamber 15 to the temperature and humidity generator in real time. If the temperature and humidity inside the sample chamber 15 are lower than the preset temperature and humidity, the temperature and humidity generator is controlled to replenish the reaction medium with the preset temperature and humidity into the sample chamber 15 via the reaction medium transport device. When the temperature and humidity inside the sample chamber 15 reach the preset temperature and humidity, the temperature and humidity generator is controlled to stop working.
[0059] To ensure that the temperature and humidity sensor 40 does not affect the detection effect due to condensation caused by local low temperature, the detection value of the temperature and humidity sensor 40 is usually set to be a few degrees higher than the preset temperature and humidity value.
[0060] See Figures 1-6 As shown, the insulation medium conveying mechanism 20 includes an insulation medium input connector 21 and an insulation medium output connector 22. The housing 11 has an insulation medium inlet 115 and an insulation medium outlet 116, both of which are connected to the insulation space 16. The insulation medium input connector 21 is installed at the insulation medium inlet 115, and the insulation medium output connector 22 is installed at the insulation medium outlet 116. The insulation medium input connector 21 is used to input the insulation medium into the insulation space 16, and the insulation medium output connector 22 is used to output the insulation medium from the insulation space 16, ensuring that the insulation medium is circulated within the insulation space 16. The insulation medium can be heated by a heating mechanism to a preset temperature and then conveyed to the insulation medium input connector 21, from which it is transported into the insulation space 16.
[0061] In one embodiment, the insulation medium output connector 22 can also be connected to the heating mechanism so that the output insulation medium flows back into the heating mechanism for reheating, thereby recycling the insulation medium.
[0062] Of course, in other embodiments, a temperature sensor can also be set to monitor the temperature in the insulation space 16 in real time, and the temperature sensor can be connected to the heating mechanism. The temperature detected by the temperature sensor in the insulation space 16 is fed back to the heating mechanism in real time so as to adjust the heating temperature of the heating mechanism.
[0063] The reaction medium delivery mechanism 30 includes a reaction medium input connector 31 and a reaction medium output connector 32. The housing 11 is provided with a reaction medium inlet 117 and a reaction medium outlet 118, both of which are connected to the sample chamber 15. The reaction medium input connector 31 is installed at the reaction medium inlet 117, and the reaction medium output connector 32 is installed at the reaction medium outlet 118. The reaction medium input connector 31 is used to input the reaction medium into the sample chamber 15, and the reaction medium output connector 32 is used to output the reaction medium from the sample chamber 15. During the preparation stage of the neutron reflection experiment, the reaction medium with a preset temperature and humidity generated by the temperature and humidity generator is delivered to the sample chamber 15 through the reaction medium input connector 31. After squeezing out the air in the sample chamber 15 and expelling the air from the reaction medium output connector 32, the sample chamber 15 can be filled.
[0064] In one embodiment, the reaction medium output connector 32 can also be connected to a waste gas collector, so that the air discharged from the sample chamber 15 and the reaction medium that has completed the reaction can be discharged into the waste gas collector for centralized collection.
[0065] In this application, the sample carrier assembly 10 also includes a heat insulation layer, which covers the outer surface of the housing 11 to prevent heat loss of the heat insulation medium in the heat insulation space 16 and further improve the heat insulation effect.
[0066] See Figure 2 , Figures 4-6 As shown, the housing 11 includes an inner shell 111, an outer shell 112, a first sealing plate 113, and a second sealing plate 114. The inner shell 111 is installed inside the outer shell 112 and connected to it. There is a gap between the inner shell 111 and the outer shell 112, which surrounds the sample chamber 15. The first sealing plate 113 covers one side of the inner shell 111 and the outer shell 112, and also covers one side of the gap. The second sealing plate 114 covers the other side of the inner shell 111 and the outer shell 112, and also covers the other side of the gap. The first sealing plate 113, the second sealing plate 114, and the gap enclose a heat-insulating space 16. The inlet 1111 and the outlet 1112 are respectively located on opposite sides of the inner shell 111. The inner cavity of the inner shell 111, together with the inlet window 121 and the outlet window 131, forms the sample chamber 15. The loading and unloading port penetrates the inner shell 111 and the outer shell 112. The heat-insulating layer covers the outer surface of the outer shell 112.
[0067] See Figure 7 As shown, the sample holder 14 includes a sample holder 14 and two clamping plates 142. The sample holder 14 is detachably installed in the sample chamber 15. The two clamping plates 142 cooperate with the sample holder 14 to clamp the two sides of the sample 100 respectively. The two clamping plates 142 are detachably installed on opposite sides of the sample holder 14 to clamp the two sides of the sample 100. The clamped parts are adjacent to the two sides of the sample 100 facing the inlet 1111 and the outlet 1112.
[0068] like Figure 6 As shown, a slot 151 is also provided in the sample chamber 15, and the sample holder 14 is inserted into the slot 151 to detachably connect to the sample chamber 15.
[0069] See also Figure 7 As shown, the sample holder 14 is also provided with a clearance hole 1411. The collimation position 17 is a through hole opened on the housing 11 to facilitate laser irradiation of the sample 100 for collimation. The clearance hole 1411 is used to avoid the irradiating laser. Of course, the clearance hole 1411 is also provided with a sealing element to ensure the sealing of the sample chamber 15.
[0070] In summary, the sample temperature and humidity control experimental apparatus for the neutron reflectance spectrometer provided in this embodiment, due to the coaxial offset arrangement of the incident and exit positions relative to the sample, allows the neutron beam to enter from the incident position at a preset incident angle and irradiate the sample. After reflection from the sample, the beam exits from the exit position and is captured by the neutron reflectance spectrometer. The interface structure of the sample can then be analyzed to perform neutron reflection testing. Furthermore, the circulating insulation medium within the insulation space ensures that the sample within the sample chamber is maintained under a controlled and uniform preset temperature and humidity environment for neutron reflection testing, guaranteeing the accuracy of the test results.
[0071] The above description, in conjunction with specific embodiments, provides a further detailed explanation of this application and should not be construed as limiting the specific implementation of this application to these descriptions. For those skilled in the art, several simple deductions or substitutions can be made without departing from the inventive concept of this application.
Claims
1. A sample temperature and humidity control experimental device for a neutron reflectance spectrometer, characterized in that, include: A sample carrier assembly includes a housing, an entrance window assembly, an exit window assembly, and a sample holder. The housing has an entrance port and an exit port on opposite sides. The entrance window assembly and the exit window assembly are detachably mounted on the entrance port and the exit port, respectively, to enclose a sample cavity with the housing. The sample holder is detachably mounted in the sample cavity and is used to fix the sample, with opposite sides of the sample facing the entrance window assembly and the exit window assembly, respectively. A thermal insulation space is also provided between the inner and outer walls of the housing, surrounding the sample cavity. The entrance window assembly has an entrance position, and the exit window assembly has an exit position. The entrance position and the exit position are coaxial and offset from the sample on the sample holder. A thermal insulation medium conveying mechanism is connected to the thermal insulation space and is used to circulate and convey thermal insulation medium into the thermal insulation space. A reaction medium delivery mechanism is connected to the sample chamber and is used to circulate a reaction medium with a preset temperature and humidity into the sample chamber.
2. The sample temperature and humidity control experimental device for a neutron reflectance spectrometer as described in claim 1, characterized in that, It also includes a temperature and humidity sensor that extends into the sample chamber and is used to detect the temperature and humidity of the reaction medium within the sample chamber.
3. The sample temperature and humidity control experimental device for a neutron reflectance spectrometer as described in claim 1, characterized in that, The entrance window assembly includes an entrance window and a first cover plate. The entrance window is installed at the entrance port. The first cover plate is detachably installed on the side of the housing where the entrance port is located and presses against the entrance window. The entrance position is located on the first cover plate. The exit window assembly includes an exit window and a second cover plate. The exit window is installed at the exit port, and the second cover plate is detachably installed on the side of the housing where the exit port is located, and presses the exit window together. The ejection position is located on the second cover plate; The entrance window, the exit window, and the housing together define the sample cavity.
4. The sample temperature and humidity control experimental device for a neutron reflectance spectrometer as described in claim 3, characterized in that, The first cover plate has a first opening at the injection position, and the second cover plate has a second opening at the emission position.
5. The sample temperature and humidity control experimental apparatus for a neutron reflectance spectrometer as described in claim 1, characterized in that, The thermal insulation medium conveying mechanism includes a thermal insulation medium input connector and a thermal insulation medium output connector. The housing is provided with a thermal insulation medium inlet and a thermal insulation medium outlet. Both the thermal insulation medium inlet and the thermal insulation medium outlet are connected to the thermal insulation space. The thermal insulation medium input connector is installed at the thermal insulation medium inlet, and the thermal insulation medium output connector is installed at the thermal insulation medium outlet. The insulation medium input connector is used to input insulation medium into the insulation space, and the insulation medium output connector is used to output the insulation medium from the insulation space.
6. The sample temperature and humidity control experimental apparatus for a neutron reflectance spectrometer as described in claim 1, characterized in that, The reaction medium delivery mechanism includes a reaction medium input connector and a reaction medium output connector. The housing is provided with a reaction medium inlet and a reaction medium outlet, both of which are connected to the sample chamber. The reaction medium input connector is installed at the reaction medium inlet, and the reaction medium output connector is installed at the reaction medium outlet. The reaction medium input connector is used to input the reaction medium into the sample chamber, and the reaction medium output connector is used to output the reaction medium from the sample chamber.
7. The sample temperature and humidity control experimental apparatus for a neutron reflectance spectrometer as described in claim 1, characterized in that, The sample carrier assembly also includes a thermal insulation layer, which covers the outer surface of the housing.
8. The sample temperature and humidity control experimental apparatus for a neutron reflectance spectrometer as described in claim 7, characterized in that, The housing includes an inner shell, an outer shell, a first sealing plate, and a second sealing plate. The inner shell is installed inside the outer shell and connected to it. There is a gap between the inner shell and the outer shell. The first sealing plate covers one side of the inner shell and the outer shell and also covers one side of the gap. The second sealing plate covers the other side of the inner shell and the outer shell and also covers the other side of the gap. The first sealing plate, the second sealing plate, and the gap together form the heat-insulating space. The insulation layer covers the outer surface of the outer shell; the inner cavity of the inner shell, together with the entrance window and the exit window, forms the sample cavity.
9. The sample temperature and humidity control experimental apparatus for a neutron reflectance spectrometer as described in claim 1, characterized in that, The outer side of the shell facing the sample is also provided with a collimation position, which is used to collimate the sample at the sample position.
10. The sample temperature and humidity control experimental apparatus for a neutron reflectance spectrometer as described in claim 1, characterized in that, The sample holder includes a base and two clamps. The base is detachably installed in the sample cavity, and the two clamps cooperate with the base to clamp the two sides of the sample respectively.