Hybrid gas temperature and humidity control device and method for neutron scattering experiments

Abstract

The application discloses a mixed gas temperature and humidity control device and method for neutron scattering experiments, which comprises a carrier gas access module, a first saturated gas providing module connected with the carrier gas access module, a second saturated gas providing module connected with the carrier gas access module, a saturated gas mixing module connected with the first saturated gas providing module, the second saturated gas providing module, the carrier gas access module and a test cavity, a heating module for heating, at least one heating point arranged on the saturated gas mixing module, a temperature monitoring module for temperature monitoring, at least one temperature monitoring point arranged on the saturated gas mixing module, and a control module capable of automatically controlling the flow of the carrier gas according to a preset total flow value, a preset temperature value, a preset humidity value and a preset humidity carrier gas ratio value, and capable of controlling the heating module to heat in real time according to the temperature monitoring value and the preset temperature value, so that the test cavity can maintain the required temperature and humidity for experiments, 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 mixed gas temperature and humidity control device and method for neutron scattering experiments. Background Technology

[0002] Neutron scattering, a key experimental method for exploring the microscopic structure and dynamic processes of matter, plays a unique role in many fields such as materials science, chemistry, and life sciences. Compared with X-rays, neutrons are not only extremely sensitive to light elements such as hydrogen, but their excellent penetrating power also makes it possible to study samples in complex environments. Therefore, developing sample environment systems that can meet the special requirements of neutron scattering has always been an important topic in this field.

[0003] Currently, temperature and humidity control in neutron scattering laboratories often employs dual-humidity and osmosis methods. The switching of the humidity equilibrium point in the dual-humidity method usually takes more than one hour, and temperature fluctuations can easily cause local condensation, thereby disrupting humidity stability. 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 current neutron scattering experiments usually takes more than 1 hour, and temperature fluctuations are prone to causing 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 mixed gas temperature and humidity control device for neutron scattering experiments, used to control the temperature and humidity inside a test chamber during neutron scattering experiments. The mixed gas temperature and humidity control device for neutron scattering experiments includes:

[0006] The carrier gas input module is used to input carrier gas and output the first, second, and third carrier gas channels.

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

[0008] The second saturated gas supply module is connected to the carrier gas access module. The second saturated gas supply module is used to access the second carrier gas and the second liquid to mix and form a second saturated gas.

[0009] A saturated gas mixing module is connected to a first saturated gas supply module, a second saturated gas supply module, a carrier gas access module, and a test chamber. The saturated gas mixing module is used to access the first saturated gas, the second saturated gas, and the third carrier gas to mix the first saturated gas, the second saturated gas, and the third carrier gas to form a mixed gas, and output the mixed gas to the test chamber.

[0010] 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;

[0011] 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 on the saturated gas mixing module.

[0012] The control module is used for:

[0013] The gas output of the first, second, and third carrier gases is controlled according to preset total flow rate, preset temperature, preset humidity, and preset wet-path carrier gas ratio. The preset wet-path carrier gas ratio is the ratio of the gas output of the first and second carrier gases. The preset total flow rate is the sum of the gas output of the first, second, and third carrier gases.

[0014] 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.

[0015] In one embodiment, the carrier gas access module includes: a first three-way valve, a second three-way valve, a first flow regulator, a second flow regulator, and a third flow regulator;

[0016] The input end of the first three-way valve is used to connect to the carrier gas, its first output end is connected to the first saturated gas supply module through the first flow regulator, and its second output end is connected to the input end of the second three-way valve.

[0017] The first output terminal of the second three-way valve is connected to the saturated gas mixing module through the second flow regulator, and its second output terminal is connected to the second saturated gas supply module through the third flow regulator.

[0018] In one embodiment, the one or more heating potentials include: a first heating point, a second heating point, and a third heating point;

[0019] The first heating point is located on the first saturated gas supply module;

[0020] The second heating point is located on the second saturated gas supply module;

[0021] The third heating point is located on the third saturated gas supply module.

[0022] In one embodiment, the one or more temperature monitoring points include: a first temperature monitoring point, a second temperature monitoring point, a third temperature monitoring point, and a fourth temperature monitoring point;

[0023] The first temperature monitoring point is set on the first saturated gas supply module;

[0024] The second temperature monitoring point is set on the second saturated gas supply module;

[0025] The third temperature monitoring point is set on the third saturated gas supply module;

[0026] The fourth temperature monitoring point is located inside the test chamber.

[0027] In one embodiment, the mixed gas temperature and humidity control device for neutron scattering experiments further includes:

[0028] 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.

[0029] In one embodiment, the mixed gas temperature and humidity control device for neutron scattering experiments further includes:

[0030] A first liquid supply module is used to supply the first liquid;

[0031] A second liquid supply module is used to supply the second liquid.

[0032] In one embodiment, the first liquid is water, and the first saturated gas supply module is a water saturator;

[0033] The second liquid is deuterated water, and the second saturated gas supply module is a deuterated water saturator.

[0034] In one embodiment, the first liquid supply module includes: a first circulation pump, a first liquid storage tank, a first liquid level sensor, a first replenishment valve, and a first replenishment pump;

[0035] The first liquid storage tank includes a first water inlet, a first water outlet, and a second water inlet; the first water inlet is connected to the first saturated gas supply module;

[0036] The inlet of the first circulating pump is connected to the first outlet, and the outlet of the first circulating pump is connected to the first saturated gas supply module; the control module is connected to the first circulating pump.

[0037] The first liquid level sensor is installed in the first liquid storage tank and is connected to the control module. The first liquid level sensor is used to monitor the liquid level in the first liquid storage tank and output a liquid level monitoring signal to the control module.

[0038] The inlet of the first replenishing pump is used to connect to a water source, and the outlet of the first replenishing pump is connected to the second inlet through the first replenishing valve.

[0039] The control module is also used to control the first replenishment pump according to the liquid level monitoring signal to replenish the first storage tank with water.

[0040] In one embodiment, the second liquid supply module includes: a second circulation pump, a second liquid storage tank, a second liquid level sensor, a second replenishment valve, and a second replenishment pump;

[0041] The second liquid storage tank includes a third water inlet, a second water outlet, and a fourth water inlet; the third water inlet is connected to the second saturated gas supply module.

[0042] The inlet of the second circulation pump is connected to the third outlet, and the outlet of the second circulation pump is connected to the second saturated gas supply module; the control module is connected to the second circulation pump.

[0043] The second liquid level sensor is installed in the second liquid storage tank and is connected to the control module. The second liquid level sensor is used to monitor the liquid level in the second liquid storage tank and output a liquid level monitoring signal to the control module.

[0044] The inlet of the second replenishing pump is used to connect to a deuterium water source, and the outlet of the second replenishing pump is connected to the fourth inlet through the second replenishing valve.

[0045] The control module is also used to control the second replenishment pump according to the liquid level monitoring signal to replenish deuterium water to the second storage tank.

[0046] According to a second aspect, one embodiment of this application provides a method for controlling the temperature and humidity of a mixed gas in a neutron scattering experiment, using the mixed gas temperature and humidity control device for a neutron scattering experiment as described above, the temperature and humidity control method comprising:

[0047] The gas output of the first carrier gas, the gas output of the second carrier gas, and the gas output of the third carrier gas are controlled according to the preset total flow rate, preset humidity, and preset wet-path carrier gas ratio.

[0048] 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.

[0049] According to the above embodiments, the mixed gas temperature and humidity control device and method for neutron scattering experiments can automatically control the gas output of the three carrier gases based on preset total flow rate, preset temperature and humidity values, and preset wet-path carrier gas ratio values ​​when maintaining the required temperature and humidity environment for the experiment. Furthermore, it can control the heating module to heat the chamber in real time based on the monitored temperature value and the preset temperature value, thereby maintaining the required temperature and humidity within the test chamber. Therefore, it is evident that temperature control can be performed in real time based on the preset temperature value and the monitored temperature value, effectively avoiding temperature fluctuations, and eliminating the need for humidity equilibrium point switching, resulting in good stability. Attached Figure Description

[0050] Figure 1 This is a schematic diagram of the connection of a mixed gas temperature and humidity control device used in a neutron scattering experiment in one embodiment;

[0051] Figure 2 This is a front view of a schematic diagram of the installation of a mixed gas temperature and humidity control device for a neutron scattering experiment on a chassis in one embodiment.

[0052] Figure 3 This is a rear view of a schematic diagram of the installation of a mixed gas temperature and humidity control device for a neutron scattering experiment on a chassis in one embodiment.

[0053] Figure 4 This is a structural diagram of the first test cavity in one embodiment;

[0054] Figure 5 This is a flowchart of a method for controlling the temperature and humidity of a mixed gas used in a neutron scattering experiment, as described in one embodiment.

[0055] Reference numerals: 10. Carrier gas supply module; 101. First three-way valve; 102. Second three-way valve; 103. First flow regulator; 104. Second flow regulator; 105. Third flow regulator; 11. First saturated gas supply module; 12. Second saturated gas supply module; 13. Saturated gas mixing module; 14. Test chamber; 141. First test chamber; 15. Constant temperature oil bath module; 16. First liquid supply module; 161. First circulating pump; 162. First liquid storage tank; 163. First liquid level sensor; 1 64. First replenishing valve; 165. First replenishing pump; 17. Second liquid supply module; 171. Second circulation pump; 172. Second storage tank; 173. Second liquid level sensor; 174. Second replenishing valve; 175. Second replenishing pump; 18. Temperature monitoring module; 181. First temperature sensor; 182. Second temperature sensor; 183. Third temperature sensor; 184. Fourth temperature sensor; 19. Control module; 191. Human-machine interface unit; 192. Main control unit; 20. Chassis; 21. Bracket. Detailed Implementation

[0056] 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.

[0057] 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.

[0058] 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).

[0059] Neutron scattering, a key experimental method for exploring the microscopic structure and dynamic processes of matter, plays a unique role in many fields such as materials science, chemistry, and life sciences. Compared with X-rays, neutrons are not only extremely sensitive to light elements such as hydrogen, but their excellent penetrating power also makes it possible to study samples in complex environments. Therefore, developing sample environment systems that can meet the special requirements of neutron scattering has always been an important topic in this field.

[0060] The significant differences in the interaction between hydrogen and its isotope deuterium with neutrons make H / D isotope substitution a powerful tool for enhancing the information content of biological neutron scattering studies across various techniques. Photons and electrons interact with atomic electric fields. Hydrogen, with only one electron, is almost invisible to X-rays. Neutrons, on the other hand, interact with the atomic nucleus, while protons have a relatively strong and negative scattering length. The isotope deuterium (D) has a stronger and positive scattering length. This difference in neutron sensitivity to hydrogen and deuterium allows isotope substitution to enhance the visibility of specific parts of complex systems. These properties form the basis for obtaining precise information about the position and dynamics of hydrogen at the atomic level using neutron scattering, while also providing unique information about large-scale, dynamic, multi-domain complexes on longer spatial and temporal scales. Comparative matching and variation achieved through careful deuteration substitution and labeling are crucial for revealing the structure of complex multi-component complexes. Neutron scattering experiments have specific requirements for deuterium water vapor. Deuterium water is expensive, and existing systems often struggle to achieve efficient utilization and precise control, which to some extent limits the development of related research.

[0061] With advancements in in-situ characterization techniques, catalysis research can now track catalyst structural evolution in real-time under actual reaction conditions. Notably, many important catalytic processes involve water vapor or hydrogen-containing atmospheres, placing extremely high demands on the precision of environmental conditions, particularly temperature and humidity control. However, while traditional neutron scattering sample environment systems can achieve high temperatures and pressures, they still face numerous technical bottlenecks in handling mixed gases, especially in systems requiring precise temperature and humidity control containing water vapor.

[0062] Currently, the dual-humidity method and the osmosis method are commonly used for temperature and humidity control. The dual-humidity method usually requires more than 1 hour to switch the humidity equilibrium point, and temperature fluctuations can easily cause local condensation, thereby destroying the stability of humidity. The osmosis method relies too heavily on the stability of key components (such as osmosis tubes) and has insufficient reliability in long-term experiments, that is, it also has the problem of poor stability.

[0063] To address the aforementioned technical problems, this application provides a mixed gas temperature and humidity control device for neutron scattering experiments, used to control the temperature and humidity inside the test chamber 14 during neutron scattering experiments.

[0064] In some embodiments, such as Figure 1 , Figure 2 and Figure 3 As shown, the mixed gas temperature and humidity control device for neutron scattering experiments may include a carrier gas access module, a first saturated gas supply module 11, a second saturated gas supply module 12, a saturated gas mixing module 13, a heating module, a temperature monitoring module 18, and a control module 19.

[0065] A carrier gas inlet module is used to receive carrier gas and output a first carrier gas, a second carrier gas, and a third carrier gas. A first saturated gas supply module 11 is connected to the carrier gas inlet module and is used to receive the first carrier gas and a first liquid to mix and form a first saturated gas. A second saturated gas supply module 12 is connected to the carrier gas inlet module and is used to receive the second carrier gas and a second liquid to mix and form a second saturated gas. A saturated gas mixing module 13 is connected to the first saturated gas supply module 11, the second saturated gas supply module 12, the carrier gas inlet module, and the test chamber 14. The saturated gas mixing module 13 is used to receive the first saturated gas, the second saturated gas, and the third carrier gas to mix and form a mixed gas, and outputs the mixed gas to the test chamber 14. A heating module is used to heat one or more heating points, at least one of which is located in the saturated gas mixing module 13. The temperature monitoring module 18 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 13.

[0066] like Figure 5 As shown, control module 19 is used to perform the following steps:

[0067] S100. Control the gas output of the first carrier gas, the gas output of the second carrier gas, and the gas output of the third carrier gas according to the preset total flow rate, preset humidity value, and preset wet-path carrier gas ratio value.

[0068] S200 receives temperature monitoring values ​​and controls the heating module to heat according to the preset temperature value and the temperature monitoring value.

[0069] In some embodiments, such as Figure 1As shown, the carrier gas access module may include a first three-way valve 101, a second three-way valve 102, a first flow regulator 103, a second flow regulator 104, and a third flow regulator 105. The input end of the first three-way valve 101 is used to access the carrier gas. The first output end of the first three-way valve 101 is connected to the input end of the first flow regulator 103 via a connecting pipe. The output end of the first flow regulator 103 is connected to the first saturated gas supply module 11 via a connecting pipe. The second output end of the first three-way valve 101 is connected to the input end of the second three-way valve 102 via a connecting pipe. The first output end of the second three-way valve 102 is connected to the input end of the second flow regulator 104 via a connecting pipe. The output end of the second flow regulator 104 is connected to the saturated gas mixing module 13 via a connecting pipe. The second output end of the second three-way valve 102 is connected to the input end of the third flow regulator 105 via a connecting pipe. The output end of the third flow regulator 105 is connected to the second saturated gas supply module 12 via a connecting pipe. Among them, the first flow regulator 103, the second flow regulator 104 and the third flow regulator 105 can all be mass flow controllers.

[0070] In some embodiments, the carrier gas may be, but is not limited to, nitrogen, and the input end of the first three-way valve 101 is connected to a nitrogen source via a connecting pipeline to access nitrogen.

[0071] In some embodiments, preset total flow rate, preset humidity, preset temperature, and preset wet-path carrier gas ratio can be determined according to experimental requirements and preset in the control module 19. The preset total flow rate is the sum of the gas output of the first, second, and third carrier gases; the preset humidity is the humidity value required for the experiment; the preset temperature is the temperature value required for the experiment; and the preset wet-path carrier gas ratio is the ratio of the gas output of the first and second carrier gases. After the preset total flow rate, preset temperature, preset humidity, and preset wet-path carrier gas ratio are determined, the control module 19 can calculate the ratio of the gas output of the wet-path carrier gas to the gas output of the dry-path carrier gas. The gas output of the wet-path carrier gas refers to the sum of the gas output of the first and second carrier gases, and the gas output of the dry-path carrier gas refers to the gas output of the third carrier gas. Therefore, once the ratio of the gas output of the wet-path carrier gas to the gas output of the dry-path carrier gas is determined, the gas output of the first, second, and third carrier gases can be determined based on the preset total flow rate, the preset wet-path carrier gas ratio, and the ratio of the gas output of the wet-path carrier gas to the gas output of the dry-path carrier gas.

[0072] During the experiment, the control module 19 controls the first flow regulator 103 according to the gas output of the first carrier gas to adjust the gas output of the first carrier gas; controls the second flow regulator 104 according to the gas output of the second carrier gas to adjust the gas output of the second carrier gas; and controls the third flow regulator 105 according to the gas output of the third carrier gas to adjust the gas output of the third carrier gas. When the first carrier gas is output to the first saturated gas supply module 11, the first saturated gas can be generated. When the second carrier gas is output to the second saturated gas supply module 12, the second saturated gas can be generated. Furthermore, by controlling the heating module to heat at least the saturated gas mixing module 13, the temperature value inside the saturated gas mixing module 13 reaches a preset temperature value, so that the temperature value of the mixed gas output from the saturated gas mixing module 13 can reach the preset temperature value, thereby ensuring that when the mixed gas is output into the test chamber 14, the temperature and humidity environment required for the experiment can be formed and maintained in the test chamber 14. Because the temperature and humidity control can be performed in real time based on preset temperature values ​​and monitored temperature values, temperature fluctuations are effectively avoided, and there is no need to switch humidity equilibrium points, resulting in good stability. This mixed gas 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, enabling precise control of the temperature and humidity environment within the test chamber 14, and precise control of the first and second saturated gases. This mixed gas temperature and humidity control device for neutron scattering experiments can be applied to in-situ neutron scattering experimental research in fields such as materials science, catalysis research, energy materials, and biomacromolecules.

[0073] In some embodiments, one or more heating points may include a first heating point, a second heating point, and a third heating point; the first heating point is disposed on the first saturated gas supply module 11; the second heating point is disposed on the second saturated gas supply module 12; and the third heating point is disposed on the saturated gas mixing module 13.

[0074] Specifically, the heating module may include a first heater, a second heater, and a third heater; the first heater is disposed on the first saturated gas supply module 11 to heat the first saturated gas supplied by the first saturated gas supply module 11; the second heater is disposed on the second saturated gas supply module 12 to heat the second saturated gas supplied by the second saturated gas supply module 12; and the third heater is disposed on the saturated gas mixing module 13 to heat the mixed gas in the saturated gas mixing module 13.

[0075] In some embodiments, the first heater, second heater, and third heater are respectively connected to the control module 19. During heating, the control module 19 can control the first heater to heat the first saturated gas supply module 11, control the second heater to heat the second saturated gas supply module 12, and control the third heater to heat the saturated gas mixing module 13, so that the temperatures of the first saturated gas supply module 11, the second saturated gas supply module 12, and the saturated gas mixing module 13 all reach the preset temperature value. The arrangement of multiple heaters allows the temperature of the mixed gas to quickly reach the preset temperature value, improving experimental efficiency and reducing temperature fluctuations.

[0076] In some embodiments, such as Figure 1 , Figure 2 As shown, the mixed gas temperature and humidity control device for neutron scattering experiments also includes a constant temperature oil bath module 15, which is used to control the temperature of the test chamber 14 so that the temperature of the test chamber 14 reaches and is dynamically maintained at a preset temperature setpoint.

[0077] Specifically, the test chamber 144 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 15 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 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.

[0078] It should be noted that, while ensuring that the temperature and humidity environment required for the experiment can be maintained within the test chamber 14, 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.

[0079] In some embodiments, one or more temperature monitoring points may include a first temperature monitoring point, a second temperature monitoring point, a third temperature monitoring point, and a fourth temperature detection point; the first temperature monitoring point is disposed on the first saturated gas supply module 11; the second temperature monitoring point is disposed on the second saturated gas supply module 12; the third temperature monitoring point is disposed on the saturated gas mixing module 13; and the fourth temperature monitoring point is disposed inside the test chamber 14.

[0080] Specifically, such as Figure 1As shown, the temperature monitoring module 18 may include a first temperature sensor 181, a second temperature sensor 182, a third temperature sensor 183, and a fourth temperature sensor 184. The first temperature sensor 181 is disposed on the first saturated gas supply module 11 as a first temperature monitoring point to monitor the temperature of the first saturated gas within the first saturated gas supply module 11. The second temperature sensor 182 is disposed on the second saturated gas supply module 12 as a second temperature monitoring point to monitor the temperature of the second saturated gas. The third temperature sensor 183 is disposed on the saturated gas mixing module 13 as a third temperature monitoring point to monitor the temperature of the mixed gas. The fourth temperature sensor 184 is disposed within the test chamber 14 as a fourth temperature monitoring point to monitor the temperature within the test chamber 14. Because temperature monitoring can be performed at multiple points, the accuracy of the temperature during the experiment is ensured.

[0081] It should be noted that in practical applications, an insulation layer is installed on the outside of the connecting pipes, and the first saturated gas supply module 11 is equipped with a first heater, the second saturated gas module is equipped with a second heater, the saturated gas mixing module 13 is equipped with a third heater, and the test chamber 14 is also equipped with a constant temperature oil bath module 15. Therefore, in practical applications, the temperature values ​​monitored by the first temperature sensor 181, the second temperature sensor 182, the third temperature sensor 183, and the fourth temperature sensor 184 can be considered to be the same value.

[0082] In some embodiments, such as Figure 1 As shown, the mixed gas temperature and humidity control device for neutron scattering experiments also includes a first liquid supply module 16 for supplying a first liquid and a second liquid supply module 17 for supplying a second liquid. The first liquid is water, and the first saturated gas supply module 11 is a water saturator; the second liquid is deuterated water, and the second saturated gas supply module 12 is a deuterated water saturator.

[0083] like Figure 1 As shown, the first liquid supply module 16 may include a first circulation pump 161, a first liquid storage tank 162, a first liquid level sensor 163, a first replenishment valve 164, and a first replenishment pump 165.

[0084] Specifically, the water saturator may include an air inlet, an air outlet, a water inlet, and a water outlet. The first liquid storage tank 162 includes a first water inlet, a first water outlet, and a second water inlet. During connection, the first inlet is connected to the outlet of the water saturator via a connecting pipe; the inlet of the first circulation pump 161 is connected to the first outlet via a connecting pipe, and the outlet of the first circulation pump 161 is connected to the inlet of the water saturator via a connecting pipe; the control module 19 is connected to the first circulation pump 161; the first liquid level sensor 163 is installed in the first storage tank 162, and the first liquid level sensor 163 is connected to the control module 19. The first liquid level sensor 163 is used to monitor the liquid level in the first storage tank 162 and outputs a liquid level monitoring signal to the control module 19; the inlet of the first replenishment pump 165 is used to connect to a water source, and the outlet of the first replenishment pump 165 is connected to the second inlet via the first replenishment valve 164; the control module 19 is also used to control the first replenishment pump 165 according to the liquid level monitoring signal to replenish water to the first storage tank 162.

[0085] In application, the control module 19 can set a first minimum liquid level threshold and a first maximum liquid level threshold. When the liquid level in the first storage tank 162, as indicated by the liquid level monitoring signal output by the first liquid level sensor 163, is the first minimum liquid level threshold, the control module 19 controls the first replenishment pump 165 and the first replenishment valve 164 to replenish water to the first storage tank 162. When the liquid level in the first storage tank 162, as indicated by the liquid level monitoring signal output by the first liquid level sensor 163, is the first maximum liquid level threshold, the control module 19 shuts down the first replenishment pump 165 and simultaneously closes the first replenishment valve 164 to stop replenishing water.

[0086] This demonstrates that automatic water replenishment can be achieved during the experiment, completely avoiding the problem of the experiment being affected by the depletion of water in the first storage tank 162 due to evaporation.

[0087] In some embodiments, the first replenishment valve 164 may be, but is not limited to, a solenoid valve.

[0088] In some embodiments, such as Figure 1As shown, the second liquid supply module 17 may include a second circulation pump 171, a second liquid storage tank 172, a second liquid level sensor 173, a second replenishment valve 174, and a second replenishment pump 175. The second storage tank 172 includes a third inlet, a second outlet, and a fourth inlet; the third inlet is connected to the second saturated gas supply module 12; the inlet of the second circulation pump 171 is connected to the third outlet, and the outlet of the second circulation pump 171 is connected to the second saturated gas supply module 12; the control module 19 is connected to the second circulation pump 171; the second liquid level sensor 173 is installed in the second storage tank 172, and the second liquid level sensor 173 is connected to the control module 19. The second liquid level sensor 173 is used to monitor the liquid level in the second storage tank 172 and output a liquid level monitoring signal to the control module 19; the inlet of the second replenishment pump 175 is used to connect to a deuterium water source, and the outlet of the second replenishment pump 175 is connected to the fourth inlet through the second replenishment valve 174; the control module 19 is also used to control the second replenishment pump 175 according to the liquid level monitoring signal to replenish deuterium water to the second storage tank 172.

[0089] Specifically, a deuterium water saturator may include an air inlet, an air outlet, a water inlet, and a water outlet. During connection, the third inlet is connected to the outlet of the deuterium saturator via a connecting pipe; the inlet of the second circulation pump 171 is connected to the second outlet via a connecting pipe, and the outlet of the second circulation pump 171 is connected to the inlet of the deuterium saturator via a connecting pipe; the control module 19 is connected to the second circulation pump 171; the second liquid level sensor 173 is installed in the second storage tank 172, and the second liquid level sensor 173 is connected to the control module 19. The second liquid level sensor 173 is used to monitor the liquid level in the second storage tank 172 and outputs a liquid level monitoring signal to the control module 19; the inlet of the second replenishment pump 175 is used to connect to the deuterium water source, and the outlet of the second replenishment pump 175 is connected to the fourth inlet via the second replenishment valve 174; the control module 19 is also used to control the second replenishment pump 175 according to the liquid level monitoring signal output by the second liquid level sensor 173 to replenish deuterium water to the second storage tank 172.

[0090] In application, the control module 19 can set a second minimum liquid level threshold and a second maximum liquid level threshold. When the liquid level in the second storage tank 172, represented by the liquid level monitoring signal output by the second liquid level sensor 173, is the second minimum liquid level threshold, the control module 19 controls the second replenishment pump 175 and the second replenishment valve 174 to replenish water to the second storage tank 172. When the liquid level in the second storage tank 172, represented by the liquid level monitoring signal output by the second liquid level sensor 173, is the second maximum liquid level threshold, the control module 19 shuts down the second replenishment pump 175 and simultaneously closes the second replenishment valve 174 to stop replenishing deuterium water.

[0091] This demonstrates that automatic replenishment of deuterium water can be achieved during the experiment, completely avoiding the problem of the experiment being affected by the depletion of deuterium water in the second storage tank 172 due to evaporation. This mixed gas temperature and humidity control device for neutron scattering experiments can not only automatically replenish water but also automatically replenish deuterium water, thus enabling the experiment to continue for several days without the need for manual replenishment of deuterium water or other water.

[0092] In some embodiments, the second replenishing valve 174 may be, but is not limited to, a solenoid valve.

[0093] In some embodiments, the ratio of the gas output of the wet path carrier gas to the gas output of the dry path carrier gas can be calculated using the following formula:

[0094] ;

[0095] 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 is the ratio of the gas output of the wet-path carrier gas to the gas output of the dry-path carrier gas.

[0096] Furthermore, the gas output of the wet-path carrier gas and the gas output of the dry-path carrier gas can be determined based on the ratio of the gas output of the wet-path carrier gas to the gas output of the dry-path carrier gas. The specific calculation formula is as follows:

[0097] ;

[0098] The preset total flow rate value; This refers to the output volume of the wet-path carrier gas. The gas output of the main road carrier gas.

[0099] Once the output volume of the wet-path carrier gas is determined, the output volume of the first carrier gas and the output volume of the second carrier gas can be determined based on the preset wet-path carrier gas ratio.

[0100] In some embodiments, such as Figure 2 , Figure 3As shown, the control module 19 may include a human-machine interface unit 191 and a main control unit 192. The main control unit 192 may include a programmable logic controller, a power supply, a signal processing unit, and the human-machine interface unit 191. The power supply provides a stable and safe power supply, and its details will not be elaborated here. The signal processing unit can realize closed-loop control of data acquisition-conversion-transmission-feedback, and its details will not be elaborated here. The programmable logic controller (PLC) inputs preset parameters such as total flow rate, temperature and humidity, temperature, wet-path carrier gas ratio, first minimum liquid level threshold, first maximum liquid level threshold, second minimum liquid level threshold, and second maximum liquid level threshold into the programmable logic controller (PLC) via the human-machine interface unit 191. As the core "brain" of the mixed gas temperature and humidity control device used in neutron scattering experiments, the PLC receives instructions from the human-machine interface unit 191 and integrates feedback from various sensors (temperature sensors, heaters, etc.) to precisely operate the first circulation pump 161, first replenishing valve 164, first replenishing pump 165, second circulation pump 171, second replenishing valve 174, second replenishing pump 175, first flow regulator 103, second flow regulator 104, and third flow regulator 105. The human-machine interface unit 191 can be a touchscreen or a control panel.

[0101] In some embodiments, the saturated gas mixing module 13 can be a gas mixer, which includes a first input terminal, a second input terminal, a third input terminal, and a first output terminal. The first input terminal of the gas mixer is connected to the outlet of the water saturator via a connecting pipe. The second input terminal of the gas mixer is connected to the outlet of the deuterium-water saturator via a connecting pipe. The third input terminal of the gas mixer is connected to the output terminal of the third flow regulator 105 via a connecting pipe. The first output terminal of the gas mixer is connected to the test chamber 14 via a connecting pipe. This gas mixer can mix the first saturated gas, the second saturated gas, and the third carrier gas to form a mixed gas, which is then output to the test chamber 14.

[0102] In some embodiments, the water saturator and the deuterium water saturator can be a three-channel saturation module. The three-channel saturation module is provided with a first saturation chamber and a second saturation chamber. The first saturation chamber and the second saturation chamber are isolated from each other. The three-channel saturation module can generate a first saturation gas in the first saturation chamber and a second saturation gas in the second saturation chamber. The first liquid and the second liquid can be completely isolated from each other to prevent cross-contamination.

[0103] In some embodiments, such as Figure 4As shown, the test chamber 14 may include a first test chamber 141, which is a cavity for rapidly adjusting the temperature and humidity of the sample used in a small-angle neutron scattering spectrometer. This mixed gas temperature and humidity control device for neutron scattering experiments is based on a humidity control scheme using a dry-wet gas ratio mixing, a jacketed oil bath circulation system (constant temperature oil bath module 500), and a heating module-coordinated global temperature control strategy. With a low-absorption cavity structure optimized for neutron beam transmission and a sophisticated sample cavity design, it achieves rapid and precise adjustment and long-term stable maintenance of the temperature and humidity parameters of the sample's microenvironment.

[0104] 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.

[0105] 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.

[0106] 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.

[0107] In some embodiments, this application also provides a method for controlling the temperature and humidity of a mixed gas in a neutron scattering experiment, using the mixed gas temperature and humidity control device for neutron scattering experiments as described above, such as... Figure 5 As shown, the method for controlling the temperature and humidity of the mixed gas used in neutron scattering experiments includes the following steps:

[0108] S100. Control the gas output of the first carrier gas, the gas output of the second carrier gas, and the gas output of the third carrier gas according to the preset total flow rate, preset temperature, preset humidity, and preset wet-path carrier gas ratio.

[0109] S200: Receives temperature monitoring values ​​and controls the heating module to heat according to the preset temperature value and the monitored temperature value. This is as described in the specific embodiment of the mixed gas temperature and humidity control device for neutron scattering experiments above, and will not be elaborated further here.

[0110] 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 mixed gas temperature and humidity control device for neutron scattering experiments, used to control the temperature and humidity of the mixed gas in the test chamber during neutron scattering experiments, characterized in that, The mixed gas temperature and humidity control device for the neutron scattering experiment includes: The carrier gas input module is used to input carrier gas and output the first, second, and third carrier gas channels. The first saturated gas supply module is connected to the carrier gas access module. The first saturated gas supply module is used to access the first carrier gas and the first liquid to mix and form the first saturated gas. The second saturated gas supply module is connected to the carrier gas access module. The second saturated gas supply module is used to access the second carrier gas and the second liquid to mix and form a second saturated gas. A saturated gas mixing module is connected to a first saturated gas supply module, a second saturated gas supply module, a carrier gas access module, and a test chamber. The saturated gas mixing module is used to access the first saturated gas, the second saturated gas, and the third carrier gas to mix the first saturated gas, the second saturated gas, and the third 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 on the saturated gas mixing module. The control module is used for: The gas output of the first, second, and third carrier gases is controlled according to preset total flow rate, preset temperature, preset humidity, and preset wet-path carrier gas ratio. The preset wet-path carrier gas ratio is the ratio of the gas output of the first and second carrier gases. The preset total flow rate is the sum of the gas output of the first, second, and third carrier gases. 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 mixed gas temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The carrier gas access module includes: a first three-way valve, a second three-way valve, a first flow regulator, a second flow regulator, and a third flow regulator; The input end of the first three-way valve is used to connect to the carrier gas, its first output end is connected to the first saturated gas supply module through the first flow regulator, and its second output end is connected to the input end of the second three-way valve. The first output terminal of the second three-way valve is connected to the saturated gas mixing module through the second flow regulator, and its second output terminal is connected to the second saturated gas supply module through the third flow regulator.

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

4. The mixed gas 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, a third temperature monitoring point, and a fourth temperature monitoring point; The first temperature monitoring point is set on the first saturated gas supply module; The second temperature monitoring point is set on the second saturated gas supply module; The third temperature monitoring point is set on the third saturated gas supply module; The fourth temperature monitoring point is located inside the test chamber.

5. The mixed gas temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The mixed gas temperature and humidity control device for neutron scattering experiments 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 mixed gas temperature and humidity control device for neutron scattering experiments as described in claim 1, characterized in that, The mixed gas temperature and humidity control device for neutron scattering experiments also includes: A first liquid supply module is used to supply the first liquid; A second liquid supply module is used to supply the second liquid.

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

8. The mixed gas temperature and humidity control device for neutron scattering experiments as described in claim 7, characterized in that, The first liquid supply module includes: a first circulation pump, a first liquid storage tank, a first liquid level sensor, a first replenishment valve, and a first replenishment pump; The first liquid storage tank includes a first water inlet, a first water outlet, and a second water inlet; the first water inlet is connected to the first saturated gas supply module; The inlet of the first circulating pump is connected to the first outlet, and the outlet of the first circulating pump is connected to the first saturated gas supply module; the control module is connected to the first circulating pump. The first liquid level sensor is installed in the first liquid storage tank and is connected to the control module. The first liquid level sensor is used to monitor the liquid level in the first liquid storage tank and output a liquid level monitoring signal to the control module. The inlet of the first replenishing pump is used to connect to a water source, and the outlet of the first replenishing pump is connected to the second inlet through the first replenishing valve. The control module is also used to control the first replenishment pump according to the liquid level monitoring signal to replenish the first storage tank with water.

9. The mixed gas temperature and humidity control device for neutron scattering experiments as described in claim 7, characterized in that, The second liquid supply module includes: a second circulation pump, a second liquid storage tank, a second liquid level sensor, a second replenishment valve, and a second replenishment pump; The second liquid storage tank includes a third water inlet, a second water outlet, and a fourth water inlet; the third water inlet is connected to the second saturated gas supply module. The inlet of the second circulation pump is connected to the third outlet, and the outlet of the second circulation pump is connected to the second saturated gas supply module; the control module is connected to the second circulation pump. The second liquid level sensor is installed in the second liquid storage tank and is connected to the control module. The second liquid level sensor is used to monitor the liquid level in the second liquid storage tank and output a liquid level monitoring signal to the control module. The inlet of the second replenishing pump is used to connect to a deuterium water source, and the outlet of the second replenishing pump is connected to the fourth inlet through the second replenishing valve. The control module is also used to control the second replenishment pump according to the liquid level monitoring signal to replenish deuterium water to the second storage tank.

10. A method for controlling the temperature and humidity of a mixed gas in a neutron scattering experiment, comprising the mixed gas temperature and humidity control device for a neutron scattering experiment as described in any one of claims 1-9, characterized in that, The method for controlling the temperature and humidity of the mixed gas used in neutron scattering experiments includes: The gas output of the first carrier gas, the gas output of the second carrier gas, and the gas output of the third carrier gas are controlled according to the preset total flow rate, preset humidity, and preset wet-path carrier gas ratio. 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.

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