A solid gas target for inert gas quantitative storage and a preparation method thereof

Abstract

The application discloses a solid gas target for inert gas quantitative storage and a preparation method thereof. The solid gas target comprises a shell, a high-adsorption porous material is arranged in the shell, inert gas is adsorbed in the high-adsorption porous material, a thin tube section is connected to the top of the shell and communicates with the inside of the shell, and a sealing filler is arranged in the thin tube section. The shell is in a cylindrical shape, and the thin tube section is connected to the curved surface of the shell. The application is oriented to inert gas quantitative storage, a low-neutron-interference porous material with special adsorption capacity for inert gas is designed and synthesized as the solid gas target, on-demand forming and sealing technologies of the inert gas adsorbent are researched, and the solid gas target sample meeting neutron source testing is prepared.

Description

Technical Field

[0001] This invention relates to a gas target, specifically to a solid gas target for quantitative storage of inert gases and its preparation method. Background Technology

[0002] Neutron nuclear data are fundamental data for basic nuclear physics research, nuclear energy development and utilization, and nuclear technology development. With the increasing sophistication of nuclear device research and the development of new advanced nuclear energy systems, nuclear data research has entered a high-precision era. The precision of existing nuclear data for related nuclides, especially inert gas nuclides, is far from meeting the requirements. Insufficient precision of reaction cross-sections for important nuclides and the lack of yield data for important nuclides mean that existing gaseous nuclide data cannot meet the needs of nuclear device research and advanced nuclear energy system development under the new circumstances.

[0003] The key elements for improving the accuracy of gaseous nuclide nuclear data measurement experiments are neutron sources, detectors, measurement methods, and gas target sample preparation techniques. In recent years, significant progress has been made in neutron source construction, high-precision detector development, and research into novel data measurement methods. However, research progress in target matrix and target preparation techniques, especially high-precision quantitative target preparation techniques for gaseous targets, has been slow, and a systematic technological accumulation has not yet been formed. As the range of nuclides to be measured expands from traditional solid metal elements to gaseous elements, the accurate measurement of nuclear data has created a clear demand for the development of high-abundance solid-state gaseous targets. Summary of the Invention

[0004] The purpose of this invention is to provide a solid gas target material for quantitative storage of inert gases and its preparation method, so as to solve the current problems of high difficulty and poor quantitative accuracy in inert gas target preparation. Guided by the quantitative storage of inert gases, this invention designs and synthesizes a low neutron interference porous material with special adsorption capacity for inert gases as a solid gas target material, studies the on-demand molding and sealing technology of inert gas adsorbents, and prepares solid gas target samples that meet the requirements of neutron source testing.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] A solid gas target for quantitative storage of inert gas includes a shell, wherein a high-adsorption-capacity porous material is disposed inside the shell, the high-adsorption-capacity porous material adsorbs inert gas, a thin tube segment is connected to the top of the shell and communicates with the interior of the shell, and a sealing filler is disposed in the thin tube segment;

[0007] The shell is cylindrical, and the thin tube segment is connected to the curved surface of the shell.

[0008] Furthermore, the housing is made of quartz.

[0009] Furthermore, the high-adsorption-capacity porous material is activated carbon; the sealing filler is EVA resin.

[0010] A method for preparing a solid gas target for quantitative storage of inert gases includes the following steps:

[0011] 1) Add a high-adsorption-capacity porous material to the shell, install a cotton filter inside the thin tube section at the upper end of the shell, connect the shell containing the high-adsorption-capacity porous material to the injection tube containing the sealing filler through a valve, connect the top of the injection tube containing the sealing filler to the adsorption instrument through a thread, open the valve, and use the adsorption instrument to evacuate the shell, thin tube section and injection tube, and heat the shell to activate the high-adsorption-capacity porous material inside it.

[0012] 2) Close the valve and maintain the vacuum below the valve. Remove the part below the threaded port and weigh it to obtain the total weight when the shell is under vacuum and record it as m1.

[0013] 3) After weighing, reconnect the adsorbent, evacuate the vacuum again, fill the adsorbent with the inert gas to be adsorbed, open the valve and perform gas adsorption equilibrium under the preset pressure.

[0014] 4) After adsorption equilibrium is reached, close the valve, remove the part below the threaded end and weigh it to obtain the total weight of the target material when it is filled with inert gas and record it as m2;

[0015] 5) After weighing twice, reconnect the adsorption instrument, heat the sealing filler to melt it into liquid, open the valve and let the liquid flow down to fill the thin tube section;

[0016] 6) Stop heating and wait at room temperature for the hot-melted sealing filler to solidify again to obtain an inert gas solid gas target.

[0017] Furthermore, the valve is made of polytetrafluoroethylene; the injection tube is made of quartz.

[0018] Furthermore, in step 1), the heating temperature is 120°C and the heating time is 1 hour.

[0019] Furthermore, in step 3), the preset pressure is 8 bar and the adsorption equilibrium time is 15 min.

[0020] Furthermore, in step 5), the heating temperature is 80°C.

[0021] Furthermore, the adsorption mass of the inert gas in the inert gas solid gas target is m. 吸附气 Body = m2 - m1;

[0022] Where, m1 = m 密封填充物 +m 注胶管 +m 阀门 +m壳体 m2 = m 密封填充物 +m 注胶管 +m 阀门 +m 壳体 +m 吸附气体 ;m 密封填充物 For the mass of the sealing filler, m 注胶管 For the quality of the dispensing tubing, m 阀门 For the mass of the valve, m 壳体 The mass of the shell.

[0023] Furthermore, in step 3), when the inert gas to be adsorbed is introduced into the adsorption instrument, the shell portion is immersed in a liquid nitrogen or ethanol cryogenic bath.

[0024] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0025] This invention designs an in-situ activation-adsorption-thermal melting curing device. By switching the valves, the mass change before and after adsorption, i.e. the mass of the adsorbed inert gas, can be accurately obtained, effectively overcoming the previous shortcomings of difficulty in quantitatively filling the gas. The use of a sealing filler with thermal melting properties can simultaneously meet the dual requirements of filling inert gas through the gaps in the sealing filler during adsorption and turning it into a liquid during sealing to prevent gas leakage, thus improving the ease of operation and the stability of the solid gaseous target.

[0026] This invention provides a valve-controlled in-situ activation-adsorption-thermal curing device for quantitative determination and encapsulation. It employs a method of equilibrating the adsorption of inert gases by porous materials with high adsorption capacity at low temperatures, followed by thermal curing with injected resin materials, to produce quartz-shelled inert gas targets with precise quantitative determination and stable performance. This achieves high storage capacity while ensuring extremely low leakage rates, and is characterized by simple operation, good repeatability and reproducibility. It also reduces interference from the target matrix on the measured signal, forming a systematic and mature high-precision quantitative target preparation technology for gas targets. This provides new ideas and methods for research in neutron source construction, high-precision detector development, and novel data measurement methods. Attached Figure Description

[0027] The accompanying drawings are provided to further understand the invention and constitute a part of this invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an improper limitation of the invention.

[0028] Figure 1 This is a schematic diagram of the structure of the present invention.

[0029] Figure 2 These are embodiments of the present invention, wherein (a) is a connection diagram and (b) is an operation diagram.

[0030] The components are: 1. shell; 2. porous material with high adsorption capacity; 3. thin tube section. Detailed Implementation

[0031] To enable those skilled in the art to better understand the present invention, the technical solution of the present invention will be further described in detail below with reference to the accompanying drawings. The description is for explanation and not limitation of the present invention.

[0032] It should be noted that the terms "comprising" and "having" and any variations thereof in the specification and claims of this invention are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or units is not necessarily limited to those steps or units that are explicitly listed, but may include other steps or units that are not explicitly listed or that are inherent to such processes, methods, products, or devices.

[0033] Example

[0034] This invention provides a solid gas target material for quantitative storage of inert gases, such as... Figure 1 As shown, the target includes a shell 1, a high-adsorption-capacity porous material 2, and a thin tube segment 3. Before adsorption, the high-adsorption-capacity porous material 2 is loaded into the shell 1 of the target. After adsorption, the inert gas is sealed in the target by the sealing filler pre-placed in the thin tube segment 3.

[0035] The shell 1 is cylindrical and made of quartz. In this example, the radius of shell 1 is 10 mm, the thickness is 10 mm, and the wall thickness is 1 mm.

[0036] High-adsorption-capacity porous material 2 uses activated carbon.

[0037] The sealing filler is made of EVA resin material.

[0038] A method for preparing a solid gas target for quantitative storage of inert gases includes the following steps:

[0039] 1) In Figure 1 The cylindrical portion of the housing 1 shown is first filled with a high-adsorption-capacity porous material 2. A cotton filter element is installed in the thin tube section 3 at the upper end of the housing 1. The housing 1 containing the high-adsorption-capacity porous material 2 is then connected to the valve and the injection tube containing the sealing filler, as shown in the diagram. Figure 2 Connect the shown connection, then connect the adsorption instrument via a threaded connection, open the valve, evacuate the vacuum, and heat at 120°C to activate the high-adsorption porous material for 2 hours.

[0040] 2) Close the valve and maintain vacuum below the valve. Remove the part below the threaded port and weigh it. The total weight of the housing 1 under vacuum is obtained at this time, denoted as m1: m1 = m 密封填充物 +m 注胶管 +m 阀门 +m 靶材 ;

[0041] 3) After weighing, reconnect the adsorbent as in step 1, evacuate the vacuum again, and fill the adsorbent with the inert gas to be adsorbed (xenon is used in this embodiment). Open the valve and perform gas adsorption equilibrium at 8 bar for 15 minutes.

[0042] 4) After adsorption equilibrium is reached, close the valve, remove the part below the threaded opening, and weigh it. This gives the total weight of shell 1 when it is filled with inert gas, denoted as m2: m2 = m 密封填充物 +m 注胶管 +m 阀门 +m 靶材 +m 吸 Gas attached;

[0043] 5) After the second weighing, reconnect the adsorption instrument as in step 1, heat the sealing filler to 80°C to melt it into a clear and transparent liquid, open the valve and let the liquid flow down to fill the thin tube section above the shell 1.

[0044] 6) After stopping heating, wait at room temperature for the sealed liquid after the heat fusion to solidify again into a solid, and an inert gas solid gas target material is produced.

[0045] Final adsorbed gas mass: m 吸附气体 =m2-m1.

[0046] Low-temperature adsorption can significantly increase the gas storage capacity of inert gas targets. This invention provides a valve-controlled in-situ activation-adsorption-thermal melting curing device. First, the shell 1 is connected to the adsorbent for degassing and activation, obtaining an initial mass under vacuum. The shell 1 is then reconnected to the adsorbent, partially immersed in a liquid nitrogen or ethanol low-temperature bath, and filled with adsorbed gas. After adsorption equilibrium is reached, the mixture is heated to 80°C, causing the sealing filler to melt into a clear liquid. Heating is then stopped, and the sealed liquid is allowed to solidify again at room temperature to complete the sealing process. The mass of the inert gas can be calculated by weighing the entire device after sealing. This invention utilizes a quantitative mass method to accurately analyze the amount of inert gas adsorbed by the target material.

[0047] The technical specifications of the quantitative xenon gas storage target product obtained by this invention are as follows:

[0048] Properties Internal pressure of the target material, bar Xenon content, g Xenon gas dispersion density, g / mL Black solid quartz sputtering material 0.8081 1.12 0.2676

[0049] The quality monitoring results of the quantitative storage xenon gas target material prepared by this invention are shown in the table below. The uniformity and stability of the quality prove that the target material has an extremely low leakage rate and very stable performance.

[0050] Monitoring time 2022.10.28 2022.10.29 2022.10.30 2022.11.1 2022.11.5 2022.11.20 2022.12.15 Mass, g 11.1435 11.1436 11.1435 11.1436 11.1434 11.1435 11.1435

[0051] The gas target material of this invention is used for neutron source construction, high-precision detector development, and novel data measurement. It features precise quantitative analysis, stable performance, high storage capacity while ensuring extremely low leakage rate, and is easy to operate with good repeatability and reproducibility.

[0052] As is known from common technical knowledge, this invention can be implemented through other embodiments that do not depart from its spirit or essential characteristics. Therefore, the disclosed embodiments described above are merely illustrative in all respects and are not the only ones. All modifications within the scope of this invention or equivalent to the scope of this invention are included in this invention.

Claims

1. A method for preparing a solid gas target for quantitative storage of inert gases, characterized in that, The solid gas target material for quantitative storage of inert gas includes a shell (1), a high adsorption capacity porous material (2) is disposed inside the shell (1), the high adsorption capacity porous material (2) adsorbs inert gas, a thin tube segment (3) is connected to the top of the shell (1), and the thin tube segment (3) communicates with the inside of the shell (1), and a sealing filler is disposed in the thin tube segment (3); The shell (1) is cylindrical, and the thin tube segment (3) is connected to the curved surface of the shell (1); The preparation method includes the following steps: 1) Add high adsorption capacity porous material (2) to the shell (1), install cotton filter inside the thin tube section (3) at the upper end of the shell (1), connect the shell (1) containing high adsorption capacity porous material (2) to the injection tube containing sealing filler through a valve, connect the top of the injection tube containing sealing filler to the adsorption instrument through a thread, open the valve, and use the adsorption instrument to evacuate the shell (1), thin tube section (3) and injection tube, and heat the shell to activate the high adsorption capacity porous material (2) inside it; 2) Close the valve and maintain the vacuum below the valve. Remove the part below the threaded port and weigh it to obtain the total weight of the shell (1) when the inside is under vacuum and record it as m1; 3) After weighing, reconnect the adsorbent, evacuate the vacuum again, fill the adsorbent with the inert gas to be adsorbed, open the valve and perform gas adsorption equilibrium under the preset pressure. 4) After adsorption equilibrium is reached, close the valve, remove the part below the threaded end and weigh it to obtain the total weight of the target material when it is filled with inert gas and record it as m2; 5) After weighing twice, reconnect the adsorption instrument, heat the sealing filler to melt it into liquid, open the valve and let the liquid flow down to fill the thin tube section; 6) Stop heating and wait at room temperature for the hot-melted sealing filler to solidify again to obtain an inert gas solid gas target.

2. The method for preparing a solid gas target for quantitative storage of inert gas according to claim 1, characterized in that, The valve is made of polytetrafluoroethylene; the injection tube is made of quartz.

3. The method for preparing a solid gas target for quantitative storage of inert gas according to claim 1, characterized in that, In step 1), the heating temperature is 120℃ and the heating time is 1 hour.

4. A method for preparing a solid gas target for quantitative storage of inert gas according to claim 1, characterized in that, In step 3), the preset pressure is 8 bar and the adsorption equilibrium time is 15 min.

5. The method for preparing a solid gas target for quantitative storage of inert gas according to claim 1, characterized in that, The heating temperature in step 5) is 80℃.

6. The method for preparing a solid gas target for quantitative storage of inert gas according to claim 1, characterized in that, The adsorbed mass of inert gas in the inert gas solid gas target is m. 吸附气体 =m2-m1; Where, m1=m 密封填充物 +m 注胶管 +m 阀门 +m 壳体 m2=m 密封填充物 +m 注胶管 +m 阀门 +m 壳体 +m 吸附气体 m 密封填充物 For the mass of the sealing filler, m 注胶管 For the quality of the dispensing tubing, m 阀门 For the mass of the valve, m 壳体 The mass of the shell.

7. The method for preparing a solid gas target for quantitative storage of inert gas according to claim 1, characterized in that, In step 3), when the inert gas to be adsorbed is introduced through the adsorption instrument, the shell (1) is partially immersed in a liquid nitrogen or ethanol low-temperature bath.

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