Humidity control device and method for neutron scattering experiments

Abstract

The application discloses a temperature and humidity control device and method for a neutron scattering experiment, which comprises a carrier gas access module, a saturated gas providing module, a saturated gas mixing module, a heating module and a temperature monitoring module. The carrier gas access module is used for accessing carrier gas and outputting first carrier gas and second carrier gas. The saturated gas providing module is connected with the carrier gas access module and a liquid providing module. The saturated gas mixing module is connected with the saturated gas providing module, the carrier gas access module and a test cavity. The heating module is used for heating one or more heating points, and at least one of the one or more heating points is arranged in the saturated gas mixing module. The temperature monitoring module is used for temperature monitoring at one or more temperature monitoring points. The control module can automatically control the flow of the carrier gas according to a preset total flow value, a preset temperature value and a preset temperature and humidity value, and can control the heating module to heat in real time according to a temperature monitoring value and the preset temperature value, so that the temperature and humidity required by the experiment can be maintained in the test cavity, the temperature fluctuation is effectively avoided, the humidity balance point switching is not needed, and the stability is good.

Description

Technical Field

[0001] This invention relates to the field of neutron scattering experimental technology, and specifically to a temperature and humidity control device and method for neutron scattering experiments. Background Technology

[0002] Neutron scattering, with its sensitivity to hydrogen, high penetration, and non-destructive detection characteristics, has become a powerful tool for exploring the nanoscale structure of materials, playing an increasingly important role in materials science, chemistry, and life sciences. In many neutron scattering experiments, temperature and humidity, as key environmental variables, can reversibly modulate the nanostructure inside the sample (e.g., inducing the swelling of polymer films or driving the adsorption of water molecules at the interface). However, these external conditions themselves do not directly generate scattering signals; therefore, dedicated temperature and humidity control devices are necessary to achieve accurate environmental simulation.

[0003] Currently, the dual-humidity method and the infiltration method are commonly used for temperature and humidity control. The switching of the humidity equilibrium point in the dual-humidity method usually takes more than 1 hour, and temperature fluctuations can easily cause local condensation, thereby disrupting the stability of humidity. Summary of the Invention

[0004] The main technical problem solved by this invention is that the switching of the humidity equilibrium point in the dual-wet method in neutron scattering experiments usually takes more than 1 hour, and temperature fluctuations can easily cause local condensation. In the permeation method, the stability of key components is too dependent, and the reliability is insufficient in long-term experiments.

[0005] According to a first aspect, one embodiment of this application provides a temperature and humidity control device for a neutron scattering experiment, used to control the temperature and humidity inside a test chamber during a neutron scattering experiment, the temperature and humidity control device for the neutron scattering experiment comprising:

[0006] Carrier gas access module, used to access carrier gas and output the first and second carrier gas channels;

[0007] A saturated gas supply module is connected to the carrier gas inlet module and the liquid supply module. The saturated gas supply module is used to inlet the first carrier gas and the first liquid to mix and form saturated gas.

[0008] A saturated gas mixing module is connected to the saturated gas supply module, the carrier gas access module and the test chamber. The saturated gas mixing module is used to access the saturated gas and the second carrier gas to mix the saturated gas and the carrier gas to form a mixed gas, and output the mixed gas to the test chamber.

[0009] A heating module is used to heat one or more heating points, wherein at least one of the one or more heating points is disposed in the saturated gas mixing module;

[0010] A temperature monitoring module is used to monitor temperature at one or more temperature monitoring points, wherein at least one of the one or more temperature monitoring points is located in the saturated gas mixing module.

[0011] The control module is used for:

[0012] The gas output of the first carrier gas and the gas output of the second carrier gas are controlled according to a preset total flow rate, a preset temperature, and a preset humidity; the preset total flow rate is the sum of the gas output of the first carrier gas and the gas output of the second carrier gas.

[0013] The system receives the temperature monitoring value and controls the heating module to heat the device according to the preset temperature value and the temperature monitoring value.

[0014] In one embodiment, the carrier gas access module includes: a three-way valve, a first flow regulator, and a second flow regulator;

[0015] The input end of the three-way valve is used to connect to the carrier gas, its first output end is connected to the saturated gas supply module through the first flow regulator, and its second output end is connected to the saturated gas mixing module through the second flow regulator.

[0016] In one embodiment, the carrier gas access module further includes: a first regulating valve and a second regulating valve;

[0017] The first regulating valve is located on the connection line between the first flow regulator and the saturated gas supply module;

[0018] The second regulating valve is located on the connection line between the second flow regulator and the saturated gas mixing module.

[0019] In one embodiment, the one or more heating points include: a first heating point and a second heating point; the first heating point is disposed on the saturated gas supply module; and the second heating point is disposed on the saturated gas mixing module.

[0020] In one embodiment, the one or more temperature monitoring points include: a first temperature monitoring point, a second temperature monitoring point, and a third temperature monitoring point;

[0021] The first temperature monitoring point is set on the saturated gas supply module;

[0022] The second temperature monitoring point is set on the saturated gas mixing module;

[0023] The third temperature monitoring point is located inside the test chamber.

[0024] In one embodiment, the temperature and humidity control device for the neutron scattering experiment further includes:

[0025] The constant temperature oil bath module is used to keep the test chamber warm, so that the temperature inside the test chamber reaches and is dynamically maintained at a preset temperature set point.

[0026] In one embodiment, the temperature and humidity control device for neutron scattering experiments further includes: a liquid supply module for supplying the first liquid; the first liquid is water; and the saturated gas supply module is a water saturator.

[0027] In one embodiment, the liquid supply module includes: a circulation pump and a water storage tank;

[0028] The water storage tank includes a first inlet and a first outlet; the first inlet is connected to the saturated gas supply module.

[0029] The inlet of the circulating pump is connected to the first outlet, and the outlet of the circulating pump is connected to the saturated gas supply module; the control module is connected to the circulating pump.

[0030] In one embodiment, the water storage tank further includes a second water inlet;

[0031] The liquid supply module also includes: a liquid level sensor, a water supply valve, and a water supply pump;

[0032] The liquid level sensor is installed in the water storage tank and is connected to the control module. It is used to monitor the liquid level in the water storage tank and output a liquid level monitoring signal to the control module.

[0033] The water inlet of the water pump is used to connect to a water source, and the water outlet of the water pump is connected to the second water inlet through the water supply valve;

[0034] The control module is also used to control the water replenishment pump according to the liquid level monitoring signal to replenish the water storage tank.

[0035] According to a second aspect, one embodiment of this application provides a temperature and humidity control method for a neutron scattering experiment, which applies the temperature and humidity control device for a neutron scattering experiment as described above. The temperature and humidity control method includes:

[0036] The gas output of the first carrier gas and the gas output of the second carrier gas are controlled according to the preset total flow rate, preset temperature, and preset humidity values.

[0037] The system receives temperature monitoring values ​​and controls the heating module based on preset temperature values ​​and the monitored temperature values.

[0038] According to the temperature and humidity control device and method for neutron scattering experiments described in the above embodiments, when maintaining the required temperature and humidity environment for the experiment, the flow rates of the two carrier gases can be automatically controlled based on preset total flow rate, preset temperature value, and preset temperature and humidity values. Furthermore, the heating module can be controlled in real-time based on the temperature monitoring value and the preset temperature value to maintain the required temperature and humidity within the test chamber. Therefore, when controlling temperature and humidity, real-time temperature control based on preset temperature values ​​and temperature monitoring values ​​effectively avoids temperature fluctuations and eliminates the need for humidity equilibrium point switching, resulting in good stability. Attached Figure Description

[0039] Figure 1 This is a schematic diagram of the connection of a temperature and humidity control device used in a neutron scattering experiment in one embodiment;

[0040] Figure 2 This is a front view of a schematic diagram of the installation of a temperature and humidity control device for a neutron scattering experiment in one embodiment;

[0041] Figure 3 This is a rear view of a schematic diagram of the installation of a temperature and humidity control device for a neutron scattering experiment in one embodiment.

[0042] Figure 4 This is a structural diagram of the first test cavity in one embodiment;

[0043] Figure 5 This is a structural diagram of the second test cavity in one embodiment;

[0044] Figure 6 This is a structural diagram of the third test cavity in one embodiment;

[0045] Figure 7 This is a flowchart of a temperature and humidity control method for a neutron scattering experiment in one embodiment.

[0046] Reference numerals: 10, chassis; 20, bracket; 100, carrier gas inlet module; 101, three-way valve; 102, first flow regulator; 103, second flow regulator; 200, saturated gas supply module; 300, saturated gas mixing module; 400, test chamber; 401, first test chamber; 402, second test chamber; 403, third test chamber; 500, constant temperature oil bath module; 600, liquid supply module; 601, circulating pump; 602, water storage tank; 603, water supply valve; 604, water supply pump; 605, liquid level sensor; 700, temperature monitoring module; 701, first temperature sensor; 702, second temperature sensor; 703, third temperature sensor; 800, control module; 801, human-machine interface unit; 802, main control unit. Detailed Implementation

[0047] The present invention will now be described in further detail with reference to specific embodiments and accompanying drawings. Similar elements in different embodiments are referred to by associated similar element reference numerals. In the following embodiments, many details are described to facilitate a better understanding of this 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 this application are not shown or described in the specification. This is to avoid obscuring the core parts of this 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.

[0048] Furthermore, the features, operations, or characteristics described in the specification can be combined in any suitable manner to form various embodiments. At the same time, the steps or actions in the method description can be rearranged or adjusted in a manner obvious to those skilled in the art. Therefore, the various orders in the specification and drawings are only for the clear description of a particular embodiment and do not imply a necessary order, unless otherwise stated that a particular order must be followed.

[0049] 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. Unless otherwise specified, the terms "connection" and "linkage" used in this application include both direct and indirect connections (linkages).

[0050] Neutron scattering, with its sensitivity to light elements, high penetration capability, and non-destructive detection characteristics, has become a powerful tool for exploring the nanoscale structure of materials, playing an increasingly important role in materials science, chemistry, and life sciences. In many neutron scattering experiments, temperature and humidity, as key environmental variables, can reversibly modulate the nanostructure inside the sample (e.g., inducing the swelling of polymer films or driving the adsorption of water molecules at the interface). However, these external conditions themselves do not directly generate scattering signals; therefore, dedicated temperature and humidity control devices are necessary to achieve accurate environmental simulation.

[0051] Currently, the dual-humidity method and the osmosis method are commonly used for temperature and humidity control. The dual-humidity method typically requires more than an hour to switch humidity equilibrium points, and temperature fluctuations can easily cause localized condensation, thus disrupting humidity stability. The osmosis method relies too heavily on the stability of key components (such as the osmosis tube), resulting in insufficient reliability in long-term experiments; in other words, it also suffers from poor stability. Furthermore, in experiments requiring several days of continuous operation, if liquid replenishment relies on manual operation, humidity fluctuations (with deviations reaching ±5%RH) can easily occur after 8 hours of continuous operation due to a decrease in liquid volume, compromising the consistency and reliability of long-term experimental data.

[0052] To address the aforementioned technical problems, this application provides a temperature and humidity control device for neutron scattering experiments, used to control the temperature and humidity within the test chamber during neutron scattering experiments. This temperature and humidity control device for neutron scattering experiments can be widely applied to in-situ neutron scattering experimental research in fields such as materials science, catalytic chemistry, biomacromolecules, and energy materials, providing a precise and controllable experimental environment for studying the microstructure and dynamic behavior of matter under specific temperature and humidity conditions.

[0053] In some embodiments, such as Figure 1 , Figure 2 and Figure 3 As shown, the temperature and humidity control device for neutron scattering experiments may include a carrier gas input module 100, a saturated gas supply module 200, a saturated gas mixing module 300, a heating module, a temperature monitoring module 700, and a control module 800. The carrier gas input module 100 is used to input carrier gas and output a first and a second source of carrier gas. The saturated gas supply module 200 is connected to the carrier gas input module 100 and the liquid supply module 600, and is used to input the first source of carrier gas and a first liquid to mix and form a saturated gas. The saturated gas mixing module 300 is connected to the saturated gas supply module 200, the carrier gas input module 100, and the test chamber 400, and is used to input the saturated gas and the second source of carrier gas to mix the saturated gas and carrier gas to form a mixed gas, which is then output to the test chamber 400. The heating module is used to heat one or more heating points and output temperature monitoring values; at least one of the one or more heating points is located in the saturated gas mixing module 300. The temperature monitoring module 700 is used to monitor the temperature at one or more temperature monitoring points and output the temperature monitoring value; at least one of the one or more temperature monitoring points is set in the saturated gas mixing module 300.

[0054] like Figure 7 As shown, the control module 800 is used to perform the following steps:

[0055] S100. Control the gas output of the first carrier gas and the gas output of the second carrier gas according to the preset total flow rate, preset temperature, and preset humidity values.

[0056] S200 receives temperature monitoring values ​​in real time and controls the heating module to heat according to the preset temperature value and the temperature monitoring value.

[0057] In some embodiments, such as Figure 1As shown, the carrier gas access module 100 may include a three-way valve 101, a first flow regulator 102, and a second flow regulator 103; the input end of the three-way valve 101 is used to access the carrier gas, its first output end is connected to the saturated gas supply module 200 through the first flow regulator 102, and its second output end is connected to the saturated gas mixing module 300 through the second flow regulator 103.

[0058] Specifically, the input end of the three-way valve 101 is connected to a carrier gas supply source via a connecting pipe to receive carrier gas. One output end of the three-way valve 101 (i.e., the first output end) is connected to the input end of the first flow regulator 102 via a connecting pipe, and the output end of the first flow regulator 102 is connected to the saturated gas supply module 200 via a connecting pipe; the other output end of the three-way valve 101 (i.e., the second output end) is connected to the input end of the second flow regulator 103 via a connecting pipe, and the output end of the second flow regulator 103 is connected to the saturated gas mixing module 300 via a connecting pipe. The control module 800 can adjust the gas output of the first carrier gas by adjusting the first flow regulator 102, and adjust the gas output of the second carrier gas by adjusting the second flow regulator 103. Both the first flow regulator 102 and the second flow regulator 103 can be mass flow controllers.

[0059] In some embodiments, the carrier gas may be, but is not limited to, nitrogen, and the input end of the three-way valve 101 is connected to a nitrogen source via a connecting pipeline to access nitrogen.

[0060] In some embodiments, preset total flow rate, preset humidity, and preset temperature values ​​can be determined according to experimental requirements and preset in the control module 800. The preset total flow rate is the sum of the gas output flow rates of the first carrier gas and the second carrier gas. Once the preset total flow rate, preset temperature, and preset humidity values ​​are determined, the control module 800 can calculate the ratio of the gas output of the first carrier gas to the gas output of the second carrier gas. During the experiment, the control module 800 can control the first flow regulator 102 and the second flow regulator 103 according to this ratio and the preset total flow rate. When the first carrier gas is output to the saturated gas supply module 200, saturated gas can be generated, theoretically achieving a relative humidity of 100%. Furthermore, by controlling the heating module to heat at least the saturated gas mixing module 300, the temperature within the saturated gas mixing module 300 reaches a preset temperature value. This ensures that the temperature of the mixed gas output from the saturated gas mixing module 300 reaches the preset temperature value, i.e., the temperature of the mixed gas output from the saturated gas mixing module 300 reaches the target temperature value required for the experiment. Consequently, when the mixed gas is output into the test chamber 400, the required temperature and humidity environment for the experiment is formed and maintained within the test chamber 400. Since temperature and humidity control can be performed in real time based on the preset temperature value and the temperature monitoring value, temperature fluctuations are effectively avoided, and there is no need for humidity equilibrium point switching, resulting in good stability. Applying this temperature and humidity control device for neutron scattering experiments can accurately generate an experimental environment with arbitrary humidity within the range of 20℃-90℃ and 10%-90%RH, thereby achieving precise control of the temperature and humidity environment within the test chamber 400.

[0061] In some embodiments, one or more heating points may include a first heating point and a second heating point; the first heating point is disposed on the saturated gas supply module 200; and the second heating point is disposed on the saturated gas mixing module 300.

[0062] Specifically, the heating module may include a first heater and a second heater; the first heater is disposed on the saturated gas supply module 200 to heat the saturated gas supplied by the saturated gas supply module 200; the second heater is disposed on the saturated gas mixing module 300 to heat the mixed gas at the location of the saturated gas mixing module 300.

[0063] Since the heating module can heat both the saturator supply module and the saturated gas mixing module 300 simultaneously, the saturated gas and carrier gas mixed in the saturated gas mixing module 300 can quickly reach the preset temperature value. That is, the temperature and humidity environment required for the experiment can be quickly formed in the test chamber 400 to improve the experimental efficiency.

[0064] In some embodiments, the first heater and the second heater are respectively connected to the control module 800. When heating, the control module 800 can control the first heater to heat the saturated gas supply module 200 and control the second heater to heat the saturated gas supply module 200, so that the temperature values ​​of the saturated gas supply module 200 and the saturated gas mixing module 300 reach the preset temperature value.

[0065] Setting up multiple heaters allows the temperature of the mixed gas to quickly reach the preset temperature value and reduces temperature fluctuations.

[0066] In some embodiments, such as Figure 1 , Figure 2 and Figure 3 As shown, the temperature and humidity control device for neutron scattering experiments also includes a constant temperature oil bath module 500, which is used to control the temperature of the test chamber 400 so that the temperature of the test chamber 400 reaches and is dynamically maintained at a preset temperature set point.

[0067] Specifically, the test chamber 400 may include a first chamber and a second chamber; the first chamber is used for experiments; the second chamber may be arranged adjacent to the first chamber, and the first chamber is nested within the second chamber. The constant-temperature oil bath module 500 is an oil bath circulation system. In application, the temperature to be reached by the heat transfer oil in the oil bath circulation system can be preset, i.e., a preset temperature setpoint. Then, a constant-temperature and circulating oil bath environment can be formed in the second chamber through the oil bath circulation system. The specific process will not be elaborated further here. Because a constant-temperature and circulating oil bath environment is formed in the second chamber, the experimental temperature can be further guaranteed, and the experimental accuracy can be improved.

[0068] It should be noted that, while ensuring that the temperature and humidity environment required for the experiment can be maintained within the test chamber 400, those skilled in the art can determine the specific preset temperature set point according to the actual situation, and no further restrictions are imposed here.

[0069] In some embodiments, one or more temperature monitoring points may include a first temperature monitoring point, a second temperature monitoring point, and a third temperature monitoring point; the first temperature monitoring point is located in the saturated gas supply module 200; the second temperature monitoring point is located in the saturated gas mixing module 300; and the third temperature monitoring point is located in the test chamber 400.

[0070] Specifically, such as Figure 1As shown, the temperature monitoring module 700 may include a first temperature sensor 701, a second temperature sensor 702, and a third temperature sensor 703. The first temperature sensor 701 is disposed on the saturated gas supply module 200 as a first temperature monitoring point to monitor the temperature of the saturated gas supply module 200. The second temperature sensor 702 is disposed on the saturated gas mixing module 300 as a second temperature monitoring point to monitor the temperature of the saturated gas mixing module 300. The third temperature sensor 703 is disposed on the test chamber 400 as a third temperature monitoring point to monitor the temperature within the test chamber 400. The temperature monitoring values ​​output by the first temperature sensor 701, the second temperature sensor 702, and the third temperature sensor 703 are the temperature monitoring values ​​of the temperature monitoring module 700. Because temperature monitoring can be performed at multiple points, the accuracy of the temperature during the experiment is ensured.

[0071] It should be noted that in practical applications, insulation layers are installed on the outside of the connecting pipes, and the saturated gas supply module 200 is equipped with a first heater, the saturated gas mixing module 300 is equipped with a second heater, and the test chamber 400 is also equipped with a constant temperature oil bath module 500. Therefore, in practical applications, the temperature values ​​monitored by the first temperature sensor 701, the second temperature sensor 702, and the third temperature sensor 703 can be considered to be the same value.

[0072] In some embodiments, such as Figure 1 As shown, the temperature and humidity control device for neutron scattering experiments also includes a liquid supply module 600 for supplying a first liquid.

[0073] In some embodiments, the first liquid is water. For example... Figure 1 As shown, the liquid supply module 600 may include a circulation pump 601 and a water storage tank 602; the water storage tank 602 includes a first water inlet and a first water outlet; the first water inlet is connected to the saturated gas supply module 200; the water inlet of the circulation pump 601 is connected to the first water outlet, and the water outlet of the circulation pump 601 is connected to the saturated gas supply module 200; the control module 800 is connected to the circulation pump 601.

[0074] Specifically, the saturated gas supply module 200 is a water saturator, which can mix nitrogen and water to form water-saturated gas. The water saturator may include an inlet end, an outlet end, a water inlet end, and a water outlet end. When connected, the inlet end of the water saturator is connected to the output end of the first flow regulator 102 through a connecting pipe, the outlet end of the water saturator is connected to the saturated gas mixing module 300 through a connecting pipe, the water inlet end of the water saturator is connected to the outlet end of the circulating pump 601 through a connecting pipe, and the water outlet end of the water saturator is connected to the first water inlet of the water storage tank 602 through a connecting pipe.

[0075] During application, water can be continuously supplied to the water saturator through the circulating pump 601. At the same time, the water in the water saturator can flow out through the outlet of the water saturator and flow into the water storage tank 602 through the first inlet of the water storage tank 602, so that the water temperature can be evenly distributed, thereby enhancing the stability of humidity output.

[0076] Furthermore, such as Figure 1 As shown, the water storage tank 602 also includes a second water inlet; the liquid supply module 600 also includes a liquid level sensor 605, a water replenishment valve 603, and a water replenishment pump 604; the liquid level sensor 605 is disposed in the water storage tank 602, and the liquid level sensor 605 is connected to the control module 800 to monitor the liquid level in the water storage tank 602 and output a liquid level monitoring signal to the control module 800; the water inlet of the water replenishment pump 604 is used to connect to a water source, and the water outlet of the water replenishment pump 604 is connected to the second water inlet through the water replenishment valve 603; the control module 800 is also used to control the water replenishment pump 604 and the water replenishment valve 603 according to the liquid level monitoring signal to replenish water to the water storage tank 602.

[0077] Specifically, the inlet of the water pump 604 is connected to a water source via a connecting pipe, and the outlet of the water pump 604 is connected to a water supply valve 603 via a connecting pipe. The water supply valve 603 is connected to the second inlet of the water storage tank 602 via a connecting pipe. A level sensor 605 is fixedly installed inside the water storage tank 602, capable of monitoring the liquid level in the water storage tank 602 and outputting a level monitoring signal to control the control module 800. The control module 800 can set a minimum liquid level threshold and a maximum liquid level threshold. When the liquid level in the water storage tank 602, as indicated by the level monitoring signal, is at the minimum liquid level threshold, the control module 800 controls the water pump 604 and the water supply valve 603 to work together to supply water to the water storage tank 602. When the liquid level in the water storage tank 602, as indicated by the level monitoring signal, is at the maximum liquid level threshold, the control module 800 shuts down the water pump 604 and simultaneously closes the water supply valve 603, stopping the water supply.

[0078] It is evident that automatic water replenishment can be achieved during the experiment, completely avoiding the problem of the water in the water storage tank 602 being depleted due to evaporation, which would affect the experiment. This allows the experiment to continue for several days without the need for manual water replenishment.

[0079] In some embodiments, the water supply valve 603 may be, but is not limited to, a solenoid valve.

[0080] In some embodiments, the ratio of the gas output of the first carrier gas to the gas output of the second carrier gas can be calculated using the following formula:

[0081] ;

[0082] in, The preset temperature value is The preset humidity value at that time; This refers to the actual partial pressure of water vapor. The pressure inside the water saturator; The preset temperature value is The saturated water vapor pressure at that time; This represents the ratio of the flow rate of the first carrier gas to the flow rate of the second carrier gas.

[0083] Furthermore, the gas output of the first carrier gas and the gas output of the second carrier gas can be determined based on the ratio of the gas output of the first carrier gas to the gas output of the second carrier gas. The specific calculation formula is as follows:

[0084] ;

[0085] The preset total flow rate value; This refers to the gas output of the first carrier gas. This refers to the gas output of the second carrier gas.

[0086] In some embodiments, such as Figure 2 , Figure 3 As shown, the control module 800 may include a human-machine interface unit 801 and a main control unit 802. The main control unit 802 may include a programmable logic controller (PLC), a power supply, a signal processing unit, and the PLC. The power supply provides a stable and safe power supply, details of which are omitted here. The signal processing unit enables closed-loop control of data acquisition, conversion, transmission, and feedback, details of which are omitted here. The PLC writes preset total flow rate, preset temperature and humidity, preset temperature, minimum liquid level threshold, and maximum liquid level threshold to the PLC via the PLC. The PLC, as the core "brain" of the temperature and humidity control device used in neutron scattering experiments, is responsible for receiving instructions from the PLC and integrating feedback from various sensors (temperature sensors, heaters, etc.) to accurately operate the circulating pump 601, the water supply pump 604, the first flow regulator 102, the second flow regulator 103, the heater, and other actuators. The PLC may be a touchscreen or a control panel.

[0087] In some embodiments, such as Figure 2 , Figure 3As shown, the temperature and humidity control device for neutron scattering experiments can be equipped with a housing 10 and a support frame. The temperature and humidity control device for neutron scattering experiments is installed on the housing 10; the test chamber 400 is installed on the support frame. Specifically, the housing 10 can be provided with four placement layers: the constant temperature oil bath module 500 is installed on the first layer; the circulating pump 601, the water replenishment pump 604, the circulating water tank, and the water saturator are installed on the second layer; the first flow regulator 102, the second flow regulator 103, the power supply, the controller, and the signal processing unit are installed on the third layer; and the human-machine interaction unit 801 is installed on the fourth layer; wherein the first, second, third, and fourth layers are arranged sequentially from bottom to top.

[0088] In some embodiments, the saturated gas mixing module 300 may be a gas mixer, which includes a first input terminal, a second input terminal, and a first output terminal. The first input terminal of the gas mixer is connected to the outlet terminal of the water saturator via a connecting pipe. The second input terminal of the gas mixer is connected to the output terminal of a second flow regulator via a connecting pipe. The first output terminal of the gas mixer is connected to the test chamber via a connecting pipe. This gas mixer can mix the saturated gas and the carrier gas output from the second channel to form a mixed gas, which is then output to the test chamber.

[0089] In some embodiments, the test cavity 400 can be different test cavities depending on experimental requirements. For example... Figure 4 As shown, the test cavity 400 may include a first test cavity 401, which is a temperature and humidity chamber for multiple sample positions in a small-angle neutron scattering (SANS) spectrometer. To meet the temperature and humidity requirements of the SANS spectrometer, during the neutron reflection experiment, after the pulsed neutron beam is generated by the spectrometer, the optical path is first adjusted by a guiding system to precisely align it with an aluminum beam window (e.g., 2 mm thick) set on the sample cavity, and it enters the sample region at a preset incident angle. This aluminum window is made of a low-neutron-absorbing material, and its size is optimized to ensure that the neutron beam passes through completely and without obstruction. After entering the cavity, the neutron beam directly irradiates the sample to be tested, located at the center of the cavity, with an assumed thickness of 3 mm. Based on the physical mechanism of small-angle neutron scattering, the nano- or micro-scale structural inhomogeneities within the sample (such as particles, pores, or phase interfaces) cause small-angle scattering of neutrons. By collecting neutron intensity distribution data at different scattering angles, the microstructural characteristics of the sample can be further analyzed, such as particle size, interface layer thickness, and pore distribution.

[0090] To effectively improve the utilization efficiency of the neutron beam, the temperature and humidity chamber is designed with a multi-station sample holder structure, supporting the simultaneous loading of multiple samples. Combined with a quick-release mechanical module, the time required for sample replacement and chamber reconfiguration is significantly reduced. Multiple samples can undergo simultaneous temperature and humidity pre-equilibration within the chamber, and sample switching operations can be completed in just seconds to minutes. Compared to the tens of minutes replacement cycle of traditional single-sample-position devices, efficiency is significantly improved. This design allows the neutron beam time to be used to maximize effective signal acquisition, thereby significantly improving experimental throughput and equipment utilization.

[0091] A neutron beam with a specific beam size, generated by a neutron source, is incident along a fixed direction into the test cavity 400, acting on the sample placed on the sample holder. The nanoscale microstructures within the sample (e.g., particle aggregates, pores, or phase interfaces) interact with the neutrons, causing some neutrons to scatter. Because the characteristic sizes of these structures are on the nanometer to micrometer scale, the corresponding scattering signals are concentrated in a small-angle range, and the scattered neutrons exit at an angle slightly deviating from the original incident direction. These scattered neutrons are ultimately received by detectors positioned outside the cavity. By analyzing the neutron intensity distribution at different scattering angles and applying small-angle scattering theory for fitting and inversion, multiple microstructural parameters of the sample can be extracted, including particle size, morphology, and distribution characteristics, as well as density fluctuation behavior within the material. The high-performance temperature and humidity control of the cavity relies primarily on the deep integration of three core technologies:

[0092] To achieve efficient neutron signal transmission, ultra-thin aluminum windows, only 0.1 millimeters thick, are installed on both sides of the temperature and humidity chamber—the path the neutron beam must take. Aluminum is highly transparent to neutrons, with an extremely small absorption cross-section, ensuring that the intensity attenuation of the neutron beam after passing through the entire chamber is strictly controlled within 5%, thus preserving the precious scattered signal to the greatest extent. Furthermore, aluminum's inherent high-temperature resistance and resistance to moisture corrosion allow it to withstand long-term high-humidity environments.

[0093] Secondly, the main body of the temperature and humidity chamber is made of SUS304 stainless steel, featuring a unique "double-cylinder jacket" structure. The jacket serves as a circulation channel for the heat transfer oil. During operation, the constant temperature oil bath module 500 precisely controls the heat transfer oil at the set value before pumping it into the jacket. The heat transfer oil flows evenly around the inner cavity wall, and through stable heat conduction, the temperature of the sample space becomes very uniform and stable, forming a highly efficient closed-loop temperature control circuit.

[0094] Furthermore, the temperature and humidity chamber employs a bidirectional airflow humidity control and full-area anti-condensation design. For humidity control, a classic split-flow method is used: the dry carrier gas is divided into two paths. One path is transformed into 100% saturated gas through the saturated gas supply module 200, while the other path remains dry. The required humidity for the experiment is obtained by precisely adjusting the mixing ratio of these two gas paths. To prevent condensation, the temperature of the first liquid in the saturated gas supply module 200 is kept synchronized with the temperature inside the temperature and humidity chamber (i.e., consistent), eliminating errors at the source. All connecting pipes are wrapped with insulation to ensure that the carrier gas does not condense in the connecting pipes. The pipe at the outlet of the temperature and humidity chamber can also be heated to a slightly higher temperature than the preset value to prevent the outlet from becoming a condensation point, thus making the experimental data more natural, realistic, and reliable. This slight increase could be 2 degrees Celsius, 3 degrees Celsius, etc., which can be determined by those skilled in the art based on the actual situation, and will not be elaborated further here.

[0095] In some embodiments, such as Figure 5 As shown, the test chamber 400 may include a second test chamber 402, which is a cavity for rapidly adjusting the temperature and humidity of the sample used in a small-angle neutron scattering spectrometer. This temperature and humidity control device for neutron scattering experiments is based on a humidity control scheme using a dry-wet gas ratio mixing method, a jacketed oil bath circulation system (constant temperature oil bath module 500) and a heating module co-controlled global temperature control strategy, a low-absorption cavity structure optimized for neutron beam transmission, and a sophisticated sample cavity design, achieving rapid and precise adjustment and long-term stable maintenance of the temperature and humidity parameters of the sample's microenvironment.

[0096] The compact cavity design of this small-angle neutron scattering spectrometer, which allows for rapid adjustment of sample temperature and humidity, significantly improves the internal gas replacement efficiency and field distribution uniformity, thereby reducing the equilibrium time for humidity changes to the order of minutes. This makes it possible to observe rapid dynamic processes such as interfacial water adsorption. Simultaneously, the smaller internal space helps eliminate local inhomogeneities in the temperature and humidity fields and reduces the overall operational load on the environmental control system. Regarding sample design, samples with dimensions sufficient to fully cover the neutron beam spot (e.g., 15 mm wide, 3 mm maximum thickness) are used. This ensures that the neutron beam passes completely through the effective sample area and improves sampling representativeness, making it particularly suitable for high-resolution small-angle neutron scattering experiments that require continuous operation for several hours or even days.

[0097] In the experimental optical path arrangement, the neutron beam, extracted from the neutron source and shaped by the collimation system, is incident into the cavity through a specially designed low-neutron-absorbing material (such as aluminum), accurately illuminating the sample to be tested fixed on the sample holder. The beam window size is precisely calculated to completely cover the beam cross-section, avoiding signal loss caused by edge obstruction. After the neutrons interact with the nano- to micro-scale structural units (such as particles, pores, and phase interfaces) in the sample, some neutrons will undergo small-angle scattering and are ultimately captured by the neutron detector arranged outside the cavity. By systematically analyzing the spatial distribution of neutron intensity at different scattering angles, the microstructural characteristics of the sample can be deduced, including particle size and distribution, interface layer thickness, internal pore structure, and density fluctuations.

[0098] The sample is securely mounted on a sample holder at the geometric center of the cavity, its position and size optimized to ensure complete neutron beam coverage. An external jacketed oil bath circulation system (such as a constant-temperature oil circulation or water bath jacket) maintains a constant cavity wall temperature; internally, precisely temperature- and humidity-controlled gas is continuously introduced to regulate the temperature and humidity environment surrounding the sample. Both the incident and exit neutron beams pass through specialized beam windows made of low-absorption cross-section materials (such as aluminum), ensuring cavity sealing and atmosphere isolation while minimizing neutron flux loss and parasitic scattering, guaranteeing high-quality transmission of the scattered signal to the detector.

[0099] In some embodiments, such as Figure 6 As shown, the test chamber 400 may include a third test chamber 403, which is a sample temperature and humidity control chamber for a neutron reflectance spectrometer. Specifically, the pulsed neutron beam generated by the spectrometer passes through a 1 mm thick aluminum beam window at a small incident angle (e.g., 0.25° to 5°) and enters the sample chamber. This aluminum window has low neutron absorption characteristics, which can effectively control beam intensity loss; its size is specially designed to completely cover the cross-section of the neutron beam, avoiding neutron obstruction at the edge of the beam window.

[0100] The neutron beam entering the sample chamber directly irradiates the sample located at the center of the cavity. Based on the principle of neutron reflectivity measurement, the neutron beam undergoes specular reflection on the sample surface, with the reflection angle equal to the incident angle. The reflection intensity depends on the interface structure characteristics of the sample, such as film thickness and scattering length density. The reflected neutron beam is then aimed at the exit beam window at the same angle, passes through the 1 mm aluminum window again, and exits the sample chamber.

[0101] The exit-side beam window is identical in structure and material to the incident-side beam window, and also possesses low neutron absorption performance. The beam window is installed 8 mm off-center along the horizontal axis. This design ensures precise matching with the neutron reflection path, guaranteeing the complete passage of the reflected beam without offset or obstruction, thus ensuring effective signal acquisition.

[0102] In some embodiments, this application provides a temperature and humidity control method for neutron scattering experiments, applied to the temperature and humidity control device for neutron scattering experiments described above, such as... Figure 7 As shown, the temperature and humidity control method includes the following steps:

[0103] S100. Control the gas output of the first carrier gas and the gas output of the second carrier gas according to the preset total flow rate, preset temperature, and preset humidity values.

[0104] S200: Receives real-time temperature monitoring values ​​and controls the heating module based on preset temperature values ​​and the monitored temperature values. This is as described in the specific embodiment of a temperature and humidity control device for neutron scattering experiments, and will not be elaborated further here.

[0105] The above examples illustrate the present invention only to aid in understanding it and are not intended to limit the scope of the invention. Those skilled in the art can make various simple deductions, modifications, or substitutions based on the principles of this invention.

Claims

1. A temperature and humidity control device for neutron scattering experiments, used to control the temperature and humidity inside the test chamber during neutron scattering experiments, characterized in that, The temperature and humidity control device for the neutron scattering experiment includes: Carrier gas access module, used to access carrier gas and output the first and second carrier gas channels; A saturated gas supply module is connected to the carrier gas inlet module and the liquid supply module. The saturated gas supply module is used to inlet the first carrier gas and the first liquid to mix and form saturated gas. A saturated gas mixing module is connected to the saturated gas supply module, the carrier gas access module and the test chamber. The saturated gas mixing module is used to access the saturated gas and the second carrier gas to mix the saturated gas and the carrier gas to form a mixed gas, and output the mixed gas to the test chamber. A heating module is used to heat one or more heating points, wherein at least one of the one or more heating points is disposed in the saturated gas mixing module; A temperature monitoring module is used to monitor the temperature at one or more temperature monitoring points and output the temperature monitoring value; at least one of the one or more temperature monitoring points is set in the saturated gas mixing module. The control module is used for: The gas output of the first carrier gas and the gas output of the second carrier gas are controlled according to a preset total flow rate, a preset temperature, and a preset humidity; the preset total flow rate is the sum of the gas output of the first carrier gas and the gas output of the second carrier gas. The system receives the temperature monitoring value and controls the heating module to heat the device according to the preset temperature value and the temperature monitoring value.

2. The temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The carrier gas access module includes: a three-way valve, a first flow regulator, and a second flow regulator; The input end of the three-way valve is used to connect to the carrier gas, its first output end is connected to the saturated gas supply module through the first flow regulator, and its second output end is connected to the saturated gas mixing module through the second flow regulator.

3. The temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The one or more heating points include: a first heating point and a second heating point; the first heating point is disposed on the saturated gas supply module; the second heating point is disposed on the saturated gas mixing module.

4. The temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The one or more temperature monitoring points include: a first temperature monitoring point, a second temperature monitoring point, and a third temperature monitoring point; The first temperature monitoring point is set on the saturated gas supply module; The second temperature monitoring point is set on the saturated gas mixing module; The third temperature monitoring point is located inside the test chamber.

5. The temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The temperature and humidity control device for the neutron scattering experiment also includes: The constant temperature oil bath module is used to keep the test chamber warm, so that the temperature inside the test chamber reaches and is dynamically maintained at a preset temperature set point.

6. The temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The temperature and humidity control device for the neutron scattering experiment further includes a liquid supply module for supplying the first liquid.

7. The temperature and humidity control device for neutron scattering experiments as described in claim 6, characterized in that, The first liquid is water; the saturated gas supply module is a water saturator.

8. The temperature and humidity control device for neutron scattering experiments as described in claim 7, characterized in that, The liquid supply module includes: a circulation pump and a water storage tank; The water storage tank includes a first inlet and a first outlet; the first inlet is connected to the saturated gas supply module. The inlet of the circulating pump is connected to the first outlet, and the outlet of the circulating pump is connected to the saturated gas supply module; the control module is connected to the circulating pump.

9. The temperature and humidity control device for neutron scattering experiments as described in claim 8, characterized in that, The water storage tank also includes a second water inlet; The liquid supply module also includes: a liquid level sensor, a water supply valve, and a water supply pump; The liquid level sensor is installed in the water storage tank and is connected to the control module. It is used to monitor the liquid level in the water storage tank and output a liquid level monitoring signal to the control module. The water inlet of the water pump is used to connect to a water source, and the water outlet of the water pump is connected to the second water inlet through the water supply valve; The control module is also used to control the water replenishment pump according to the liquid level monitoring signal to replenish the water storage tank.

10. A method for controlling temperature and humidity in a neutron scattering experiment, using the temperature and humidity control device for a neutron scattering experiment as described in any one of claims 1-9, characterized in that, The temperature and humidity control method includes: The gas output of the first carrier gas and the gas output of the second carrier gas are controlled according to the preset total flow rate, preset temperature, and preset humidity values. The system receives temperature monitoring values ​​and controls the heating module based on preset temperature values ​​and the monitored temperature values.

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