Sample introduction device in in-situ characterization experiment and in-situ characterization experiment device

Abstract

The utility model discloses a sampling device in an in-situ characterization experiment and an in-situ characterization experiment device, and relates to the field of in-situ spectroscopy. The utility model discloses a sampling device in an in-situ characterization experiment. The sampling device comprises an annular base, a conical cavity and an electron beam receiving cavity, wherein the conical cavity extends upwards from the annular base, is gradually closed and is not sealed; and the electron beam receiving cavity is surrounded by the conical cavity and the annular base. An annular channel extending from the bottom of the conical cavity to the top of the conical cavity is arranged in the conical cavity, an annular channel air outlet is formed in the top of the conical cavity, and an annular channel air inlet is formed in the bottom of the conical cavity. Through the arrangement, the reaction rate of the in-situ characterization experiment is increased while the reaction gas is relatively intensively conveyed to the surface of the sample.

Description

Technical Field

[0001] The utility model relates to the field of in-situ spectroscopy, in particular to a sample injection device and an in-situ characterization experimental device in an in-situ characterization experiment. Background Art

[0002] In-situ characterization technology is crucial in scientific research as it allows real-time observation and recording of reactions and material changes in the actual environment of the sample. This technology provides high-resolution and high-precision data, facilitating in-depth research on the electronic structure of materials, the coordination environment atomic structure, morphological changes, and the dynamic process of reactions. In-situ characterization technology promotes the development of new materials, new catalysts, and new drugs and is widely applied in fields such as chemistry, materials science, and biology.

[0003] However, in in-situ characterization technology, precise control of reaction gases in a near-atmospheric pressure environment is a major challenge. How to precisely control the reaction gases in the reaction area on the sample surface, including gas flow rate and gas pressure control, will have a great impact on the in-situ characterization results. In a near-atmospheric pressure chamber in in-situ characterization technology, reaction gases are delivered into the chamber through a micro-leak valve. Under the catalysis of X-rays, atoms on the sample surface react chemically with gas molecules of the reaction gases, thereby exciting electrons on the material surface; then an electron beam receiving chamber is used to collect the excited electron beam current, and relevant research on material properties is carried out based on the strength of the electron signals obtained by the detector. During the process of the reaction gases from the micro-leak valve to the sample surface, the reaction gases go from the high-pressure state of the micro-leak valve to the near-atmospheric pressure chamber environment, and the volume of the reaction gases expands sharply, and the gas density drops instantaneously to a very low level, resulting in very limited reaction gases that can actually reach the reaction area (such as a sample point with a diameter of 0.3 mm), leading to a very limited amount of reaction gases actually participating in the catalytic reaction, thus limiting the effect of in-situ characterization experiments to a certain extent. Therefore, to improve the effect of in-situ characterization experiments, it is necessary to optimize the gas inlet mode of reaction gases in in-situ characterization technology and regulate the reaction gas atmosphere flow field, thereby improving the effect of in-situ characterization experiments, which has a very important impact on the entire in-situ characterization technology. Given the importance of in-situ characterization technology to the development of materials science and the importance of atmosphere control of reaction gases in a near-atmospheric pressure environment to in-situ characterization technology, how to effectively achieve precise control of reaction gases in the reaction area on the sample surface is a key technical problem urgently to be solved in the development of in-situ characterization technology and has a huge impact on further promoting the development of materials science.

[0004] In summary, there is an urgent need for a sample injection device that can deliver reaction gases more concentratedly to the sample surface. Summary of the Utility Model

[0005] To solve the above problems, the present utility model provides a sample injection device in an in-situ characterization experiment. The sample injection device in the in-situ characterization experiment includes an annular base, a conical cavity that extends upward from the annular base and gradually converges but is not sealed, and an electron beam receiving cavity surrounded by the conical cavity and the annular base inside. A ring-shaped channel extending from the bottom to the top of the conical cavity is provided in the conical cavity. An outlet of the ring-shaped channel is provided at the top of the conical cavity, and an inlet of the ring-shaped channel is provided at the bottom of the conical cavity.

[0006] In a feasible embodiment, there are two inlets of the ring-shaped channel, and the two inlets of the ring-shaped channel are centrosymmetric with the conical cavity as the center of symmetry.

[0007] In a feasible embodiment, the cross-sectional area of the ring-shaped channel gradually decreases along the extending direction of the ring-shaped channel.

[0008] In a feasible embodiment, the cross-sectional shape of the ring-shaped channel is annular, the ring width at the bottom of the ring-shaped channel is 1 - 2 mm, and the ring width at the top of the ring-shaped channel is 0.1 - 0.2 mm.

[0009] In a feasible embodiment, both the inner wall and the outer wall of the conical cavity gradually incline towards the center line of the conical cavity along the extending direction.

[0010] In a feasible embodiment, the inclination rate of the outer wall of the conical cavity is greater than the slope of the inner wall of the conical cavity.

[0011] In a feasible embodiment, an intake pipe extending towards the outside of the conical cavity is further provided at the inlet of the ring-shaped channel.

[0012] In some feasible embodiments, the length of the intake pipe is 4 - 8 mm; and / or, the radius of the intake pipe is 0.5 - 1.5 mm; and / or, the thickness of the intake pipe is 0.1 - 0.3 mm.

[0013] In a feasible embodiment, the average thickness of the outer wall of the conical cavity is 0.1 - 0.4 mm; the average thickness of the inner wall of the conical cavity is 0.1 - 0.4 mm.

[0014] In a second aspect of the present utility model, an in-situ characterization experimental device is provided, which includes the sample injection device in the in-situ characterization experiment provided in the first aspect of the present utility model, and further includes a near-ambient pressure cavity, a characterization mechanism and a sample stage provided in the near-ambient pressure cavity. The sample stage is adapted to place a sample. The annular base is provided on the characterization mechanism, and the top of the conical cavity is aligned with the sample.

[0015] The sample injection device in an in-situ characterization experiment provided by the present utility model has the following beneficial effects:

[0016] 1) By providing an annular base, a conical cavity, and an annular channel disposed within the conical cavity, the present utility model enables the pressure of the reaction gas to be reduced from a high-pressure state within the gas delivery pipe to a low-pressure state within the annular channel during the transportation of the reaction gas. At this time, the reaction gas undergoes a violent expansion, and the potential energy of the gas is converted into kinetic energy, thereby forming a reaction gas turbulent flow model with a relatively high flow rate. Secondly, while the reaction gas turbulent flow model rapidly rotates and flows within the annular channel, due to the air pressure difference within the annular channel, the reaction gas turbulent flow model flows towards the outlet of the annular channel. After the reaction gas flows out from the outlet of the annular channel, the reaction gas is rapidly ejected onto the surface of the sample. While achieving the relatively concentrated transportation of the reaction gas to the surface of the sample, it also increases the reaction rate of the in-situ characterization experiment.

[0017] 2) The present utility model adopts a setting method with two annular channel inlets, which can accelerate the flow of gas within the annular channel, thereby forming a reaction gas turbulent flow model with a relatively high flow rate. At the same time, by using two annular channel inlets, different reaction gases can be mixed, and during the rapid flow of the reaction gas, the full mixing between reaction gases with different densities is accelerated, improving the gas state uniformity of the reaction gas within the annular channel. Secondly, the use of two annular channel inlets enables the circumferential turbulence formed by the reaction gas to further confine the reaction gas from jetting out in all directions, increasing the amount of reaction gas that reacts with the sample, and forming a relatively large turbulence at the outlet of the annular channel, creating a low-pressure area at the inlet of the electron beam receiving cavity, thereby reducing the electron scattering degree of the reaction gas.

[0018] 3) The present utility model adopts a setting where the cross-sectional area of the annular channel gradually decreases, which can further compress the reaction gas, thereby continuously increasing the density of the reaction gas turbulent flow. At the same time, as the cross-sectional area of the annular channel continuously decreases, the gas flow rate and pressure obtained at the gas outlet of the reaction gas also continuously increase, which is conducive to the relatively concentrated ejection of the reaction gas onto the surface of the sample after flowing out from the outlet of the annular channel. Description of the Drawings

[0019] Figure 1 is the overall structural schematic diagram of the sample injection device in the in-situ characterization experiment of the present utility model.

[0020] Figure 2 is the side view of the overall structure of the sample injection device in the in-situ characterization experiment of the present utility model.

[0021] Figure 3 For the present utility model Figure 2 is the cross-section in the A - A direction.

[0022] Figure 4 For the present utility model Figure 2 is the cross-section in the B - B direction.

[0023] Figure 5 This is a schematic diagram of the overall structure of the in-situ characterization experimental device of the present utility model.

[0024] Reference numerals

[0025] Annular base 1

[0026] Conical cavity 2

[0027] Annular channel 21

[0028] Annular channel air outlet 22

[0029] Annular channel air inlet 23

[0030] Air inlet pipe 24

[0031] Electron beam receiving cavity 3

[0032] Electron beam receiving cavity inlet 31

[0033] Near-atmospheric pressure cavity 4

[0034] Characterization mechanism 5

[0035] Sample 6 Specific implementation mode

[0036] Next, the technical solutions in the embodiments of the present utility model will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all the embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present utility model. In the description of the present utility model, it should be noted that the orientation or positional relationship indicated by terms such as "left side", "right side", "upper side", "lower side", "above", "below", etc. is based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be construed as a limitation of the present utility model. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.

[0037] In the description of the present utility model, it should be noted that unless otherwise clearly specified and defined, the terms "installation", "connection", and "coupling" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.

[0038] In addition, in the description of the present utility model, unless otherwise stated, the meaning of "a plurality of" is two or more.

[0039] Embodiment 1

[0040] The present utility model provides a sample injection device in an in-situ characterization experiment. Refer to Figures 1 to 4, including an annular base 1, a conical cavity 2 that extends upward from the annular base 1 and gradually converges but is not sealed, and an electron beam receiving cavity 3 surrounded by the conical cavity 2 and the annular base 1 inside. A ring-shaped channel 21 extending from the bottom of the conical cavity 2 to the top of the conical cavity 2 is provided in the conical cavity 2. An annular channel air outlet 22 is provided at the top of the conical cavity 2, and an annular channel air outlet 23 is provided at the bottom of the conical cavity 2. For illustration, the shape of the conical cavity 2 is similar to an opened umbrella. The space surrounded by the umbrella under the umbrella is the electron beam receiving cavity 3. The top of the conical cavity 2 is not a traditional conical tip but an unsealed flat opening design, similar to the shape after cutting off the umbrella tip with scissors. Therefore, the external space of the conical cavity 2 and the electron beam receiving cavity 3 can be connected through the opening at the top of the conical cavity 2, and this opening is the electron beam receiving cavity inlet 31. Generally speaking, the radius of the electron beam receiving cavity inlet 31 is 0.2 - 0.7 mm, preferably 0.5 mm. During the experiment, the sample 61 is usually placed outside the conical cavity 2 and directly opposite the electron beam receiving cavity inlet 31, and the distance between the sample 61 and the electron beam receiving cavity inlet 31 can be adjusted according to different characterization experiments. During the experiment, the reaction gas enters from the annular channel air outlet 23, flows through the annular channel 21, then flows out from the annular channel air outlet 22 and flows towards the sample 61. At the same time, X-rays are also synchronously irradiated on the sample 61. Under the combined action of X-rays and the reaction gas, the sample 61 will be excited to generate an electron beam current. The generated electron beam current can be understood as the umbrella handle of the umbrella. The electron beam current moves into the electron beam receiving cavity 3 through the electron beam receiving cavity inlet 31 and is detected by the characterization mechanism 5. In addition, when the present utility model is in use, the annular channel air outlet 23 is usually externally connected to an air delivery pipeline, and the air delivery pipeline pumps the reaction gas from the air inlet through a pump body. During the transportation of the reaction gas, the pressure of the reaction gas is reduced from the high-pressure state in the air delivery pipeline to the low-pressure state in the annular channel 21. At this time, the reaction gas undergoes a violent expansion, and the potential energy of the gas is converted into the kinetic energy of the gas, thus forming a reaction gas turbulent flow model with a relatively fast flow rate. Secondly, while the reaction gas turbulent flow model rotates rapidly in the annular channel 21, due to the air pressure difference in the annular channel 21, the reaction gas turbulent flow model flows towards the annular channel air outlet 22. It can be understood that: under the combined space limitation of the inner wall and the outer wall of the conical cavity 2, the reaction gas turbulent flow model cannot expand in the radial direction of the annular channel 21, and the reaction gas turbulent flow model can only flow along the extension direction of the annular channel 21, that is Figure 3 the arrow direction in. Finally, after the reaction gas flows out from the annular channel air outlet 22, the reaction gas is jetted onto the surface of the sample 61 sharply. While achieving the relatively concentrated transportation of the reaction gas to the surface of the sample 61, it also increases the reaction rate of the in-situ characterization experiment.

[0041] In the sampling device in the in-situ characterization experiment provided by the present utility model, refer to Figures 1 to 4 , there are two annular channel air outlets 23, and these two annular channel air outlets 23 are centrosymmetric with the conical cavity 2 as the center of symmetry. For illustration, the arrangement of two annular channel air outlets 23 can accelerate the flow of gas in the annular channel 21, thereby forming a reaction gas turbulence model with a relatively fast flow rate. At the same time, using two annular channel air outlets 23 can mix different reaction gases, and during the rapid flow of the reaction gases, it accelerates the full mixing between reaction gases with different densities, improving the gas state uniformity of the reaction gases in the annular channel 21. Secondly, the arrangement of two annular channel air outlets 23 enables the turbulence in the circumferential direction formed by the reaction gases to further confine the reaction gases from spraying out in all directions, increasing the amount of reaction gases that react with the sample 61, and forming a larger turbulence at the annular channel air outlet 22, making the inlet 31 of the electron beam receiving cavity form a low-pressure area, thereby reducing the degree of electron scattering of the reaction gases.

[0042] In the sampling device in the in-situ characterization experiment provided by the present utility model, refer to Figures 1 to 4 , the cross-sectional area of the annular channel 21 gradually decreases along the extension direction of the annular channel 21, and the cross-sectional shape of the annular channel 21 is annular. For illustration, adopting the scheme of gradually reducing the cross-sectional area of the annular channel 21 can further compress the reaction gases, thereby continuously increasing the density of the turbulent reaction gas. At the same time, as the cross-sectional area of the annular channel 21 continuously decreases, the gas flow rate and pressure obtained at the outlet of the reaction gases are also continuously increasing, which is beneficial for the reaction gases to be sprayed onto the surface of the sample 61 more concentratedly after flowing out of the annular channel air outlet 22. As a supplementary illustration, the ring width at the bottom of the annular channel 21 (the maximum ring width of the annular channel 21) is 1 - 2 mm, preferably 1 mm, and the ring width at the top of the annular channel 21 (the minimum ring width of the annular channel 21) is 0.1 - 0.2 mm, preferably 0.1 mm.

[0043] In the sampling device in the in-situ characterization experiment provided by the present utility model, refer to Figure 4 , both the inner wall and the outer wall of the conical cavity 2 gradually incline towards the center line of the conical cavity 2 along the extension direction. Further, the inclination rate of the outer wall of the conical cavity 2 is greater than the slope of the inner wall of the conical cavity 2.

[0044] In the sampling device in the in-situ characterization experiment provided by the present utility model, refer to Figure 1 and Figure 2, an intake pipe 24 extending outward from the intake port to the outside of the conical cavity 2 is further provided. Further, the length of the intake pipe 24 is 4 - 8 mm, preferably 6 mm; and / or, the radius of the intake pipe 24 is 0.5 - 1.5 mm, preferably 1 mm; and / or, the thickness of the intake pipe 24 is 0.1 - 0.3 mm, preferably 0.2 mm.

[0045] In the sampling device in the in-situ characterization experiment provided by the present utility model, refer to Figure 4 , the average thickness of the outer wall of the conical cavity 2 is 0.1 - 0.4 mm, preferably 0.2 mm; the average thickness of the inner wall of the conical cavity 2 is 0.1 - 0.4 mm, preferably 0.13 mm.

[0046] Embodiment 2

[0047] This embodiment provides an in-situ characterization experiment device, refer to Figures 1 to 5 , including the sampling device in the in-situ characterization experiment as described in Embodiment 1, and further including an atmospheric pressure chamber, a characterization mechanism 5 and a sample stage 6 provided in the near-atmospheric pressure cavity 4. The sample stage 6 is suitable for placing a sample 61. The annular base 1 is provided on the characterization mechanism 5, and the top of the conical cavity 2 is aligned with the sample 61, that is, the electron beam receiving cavity inlet 31 is aligned with the sample 61. During use, the atmospheric pressure chamber maintains an atmospheric pressure state, and then reaction gas is introduced through the sampling device in the in-situ characterization experiment. At the same time, X-rays are also synchronously irradiated on the sample 61. The electron beam excited by the sample 61 enters the electron beam receiving cavity 3 through the electron beam receiving cavity inlet 31 and enters the characterization mechanism 5.

[0048] The above are only the preferred embodiments of the present utility model. It should be noted that for those of ordinary skill in the art, without departing from the technical principle of the present utility model, several improvements and substitutions can be made, and these improvements and substitutions should also be regarded as the protection scope of the present utility model.

Claims

1. An injection device in an in-situ characterization experiment, characterized in that: It includes an annular base (1), a conical cavity (2) that extends upward from the annular base (1) and gradually converges but is not sealed, and an electron beam receiving cavity (3) surrounded by the conical cavity (2) and the annular base (1) inside. A ring-shaped channel (21) extending from the bottom of the conical cavity (2) to the top of the conical cavity (2) is provided in the conical cavity (2). An outlet (22) of the ring-shaped channel is provided at the top of the conical cavity (2), and an inlet (23) of the ring-shaped channel is provided at the bottom of the conical cavity (2).

2. The sample introduction device in the in-situ characterization experiment according to claim 1, characterized in that: There are two outlets (22) of the ring-shaped channel, and these two outlets (22) of the ring-shaped channel are centrosymmetric with the conical cavity (2) as the center of symmetry.

3. The sample injection device in the in-situ characterization experiment according to claim 1, characterized in that: The cross-sectional area of the ring-shaped channel (21) gradually decreases along the extension direction of the ring-shaped channel (21).

4. The sample introduction device in the in-situ characterization experiment according to claim 3, wherein: The cross-sectional shape of the ring-shaped channel (21) is annular. The ring width at the bottom of the ring-shaped channel (21) is 1 - 2 mm, and the ring width at the top of the ring-shaped channel (21) is 0.1 - 0.2 mm.

5. The sample introduction device in the in-situ characterization experiment according to claim 1, characterized in that: Both the inner wall and the outer wall of the conical cavity (2) gradually incline towards the center line of the conical cavity (2) along the extension direction of the conical cavity (2).

6. The sample introduction device in the in-situ characterization experiment according to claim 4, characterized in that: The inclination rate of the outer wall of the conical cavity (2) is greater than the slope of the inner wall of the conical cavity (2).

7. The sample introduction device in the in-situ characterization experiment according to claim 1, characterized in that: An intake pipe (24) extending to the outside of the conical cavity (2) is further provided at the inlet (23) of the ring-shaped channel.

8. The sample introduction device in the in-situ characterization experiment according to claim 7, characterized in that: The length of the intake pipe (24) is 4 - 8 mm; and / or, the radius of the intake pipe (24) is 0.5 - 1.5 mm; and / or, the thickness of the intake pipe (24) is 0.1 - 0.3 mm.

9. The sample introduction device in the in-situ characterization experiment according to claim 1, characterized in that: The average thickness of the outer wall of the conical cavity (2) is 0.1 - 0.4 mm; the average thickness of the inner wall of the conical cavity (2) is 0.1 - 0.4 mm.

10. An in-situ characterization experimental device, comprising a sample injection device in the in-situ characterization experiment according to any one of claims 1 to 9, characterized in that: It further includes a near-atmospheric-pressure cavity (4), a characterization mechanism (5) provided in the near-atmospheric-pressure cavity (4), and a sample stage (6). The sample stage (6) is suitable for placing a sample (61); the annular base (1) is provided on the characterization mechanism (5), and the top of the conical cavity (2) is aligned with the sample (61).

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