In-situ reaction flowing liquid system

Abstract

The utility model relates to an in-situ reaction flowing liquid system which comprises a micro-flow control system, a reaction system and a vacuum system, the reaction system comprises an in-situ liquid pool, the micro-flow control system is communicated with a flow channel of the in-situ liquid pool so as to input flowing reaction liquid into the in-situ liquid pool and output reacted liquid, and the vacuum system is communicated with the in-situ liquid pool. The in-situ liquid pool is fixedly installed in the vacuum system so as to provide a vacuum sealing environment for the in-situ liquid pool through the vacuum system, and in the in-situ liquid pool, liquid is provided in a flowing form of a thin sample layer and reacts. The in-situ reaction flowing liquid system disclosed by the utility model is reliable in structure, complete in function, stable in operation and suitable for carrying out in-situ reaction and detection in an ultrahigh vacuum environment.

Description

Technical Field

[0001] The utility model relates to an in-situ reaction liquid pool, and more specifically to an in-situ reaction flowing liquid system. Background Art

[0002] In-situ detection of physical and chemical processes at the solid-liquid and solid-gas interfaces is very important for studying the principles and mechanisms of electrochemical processes and catalytic reactions and their chemical applications. The in-situ liquid reaction cell is the core device for in-situ characterization. For the detection methods of soft X-ray absorption, fluorescence emission and scattering spectroscopy, since soft X-rays are severely lost in the air, in-situ characterization needs to be carried out under ultra-high vacuum conditions. On the other hand, the sample penetration depth of soft X-rays is usually less than 2 microns, so the applicable in-situ liquid reaction cell needs to meet the conditions of being able to work under ultra-high vacuum and thin sample layers. The static liquid pool currently used to seal liquid samples usually uses a transparent silicon nitride thin window to encapsulate the liquid (the liquid content is in the microliter range), and the liquid is stationary after encapsulation. However, since X-rays have a heating effect on liquids, especially a very small amount of liquid, the heating effect is obvious, resulting in liquid loss and radiation denaturation. In addition, the sample replacement process means that the sample must be removed and re-vacuumed, and the actual operation process is time-consuming and labor-intensive. Utility Model Content

[0003] In order to solve the above problems of liquid loss and the like in the prior art, the utility model provides an in-situ reaction flowing liquid system.

[0004] According to the in-situ reaction flow liquid system of the utility model, it includes a microfluidic control system, a reaction system and a vacuum system, wherein the reaction system includes an in-situ liquid pool, the microfluidic control system is connected to the flow channel of the in-situ liquid pool to input flowing reaction liquid into the in-situ liquid pool and output reacted liquid, the in-situ liquid pool is fixedly installed in the vacuum system to provide a vacuum sealing environment for the in-situ liquid pool through the vacuum system, and in the in-situ liquid pool, the liquid is provided in the flow form of a thin sample layer and reacts.

[0005] Preferably, the microfluidic control system includes a microfluidic injection pump assembly and a liquid storage tank, wherein the microfluidic injection pump assembly is connected to the in-situ liquid tank through an inflow pipe to introduce the reaction liquid into the in-situ liquid tank, and the in-situ liquid tank is connected to the liquid storage tank through an outflow pipe to output the reacted liquid from the in-situ liquid tank.

[0006] Preferably, the microfluidic control system further comprises electromagnetic on-off valves, which are respectively arranged on the inflow and outflow pipelines to control the on-off of the liquid.

[0007] Preferably, the microfluidic control system further comprises a flow sensor and a pressure sensor, which are respectively arranged on the inflow pipeline to monitor the real-time flux and fluid pressure of the fluid flow.

[0008] Preferably, the microfluidic control system also includes a controller and a computer, wherein the controller is connected to the electromagnetic on-off valve, flow sensor and pressure sensor through control lines to control the on-off of the electromagnetic valve and read sensor data, and the computer is connected to the controller to operate and display the controller.

[0009] Preferably, the reaction system further comprises an electrode, which is mounted on the in-situ liquid pool and inserted into the flow channel so that the reaction liquid in the flow channel undergoes an electrolytic reaction.

[0010] Preferably, the reaction system further comprises a silicon nitride window and a rubber sealing O-ring, and the silicon nitride window is pressed against the in-situ liquid pool by the rubber sealing O-ring to achieve sealing.

[0011] Preferably, the silicon nitride window has a window for X-rays to pass through.

[0012] Preferably, the inner diameter of the rubber sealing O-ring is larger than the diameter of the flow channel, and the window is located at the center of the rubber sealing O-ring.

[0013] Preferably, the vacuum system comprises a vacuum chamber for providing a vacuum environment for the in-situ liquid pool.

[0014] The in-situ reaction flowing liquid system of the utility model has a reliable structure, complete functions, and stable operation, and is suitable for in-situ reaction and detection in an ultra-high vacuum environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a structural schematic diagram of an in-situ reaction flowing liquid system according to a preferred embodiment of the utility model.

[0016] Figure 2 yes Figure 1 A partial enlarged view of .

[0017] Figure 3 yes Figure 1 Front view of the reaction system.

[0018] Figure 4 The figure shows the real-time monitoring readings of the flow sensor of the in-situ liquid pool when the microfluidic injection pump is operating normally.

[0019] Figure 5 The test results of two flow rate mutations are shown. The solenoid valve can respond quickly to the flow rate mutation and actively close to avoid liquid leakage. DETAILED DESCRIPTION

[0020] The preferred embodiments of the present utility model are given below in conjunction with the accompanying drawings and described in detail.

[0021] like Figure 1As shown, according to a preferred embodiment of the utility model, the in-situ reaction flow liquid system includes a microfluidic control system 1, a reaction system 2 and a vacuum system 3, wherein the microfluidic control system 1 is connected to the reaction system 2 to input the flowing reaction liquid into the reaction system 2 and output the liquid after the reaction, and the reaction system 2 is fixedly installed in the vacuum system 3 to provide an ultra-high vacuum sealing environment for the reaction system 2 through the vacuum system 3. In the reaction system 2, the liquid is provided in the form of a thin sample layer, and the heating effect of the X-ray on the liquid is not obvious, thereby avoiding the damage problem of the static liquid pool detection in the prior art. Moreover, since the liquid is provided in a flowing form, the sample replacement process does not require re-vacuuming and other operations, which is convenient and quick.

[0022] The microfluidic control system 1 includes a microfluidic injection pump assembly 11, a pipeline 12 and a liquid reservoir 13, wherein the microfluidic injection pump assembly 11 is connected to the reaction system 2 through the inflow pipeline 12 to introduce the reaction liquid into the reaction system 2, and the reaction system 2 is connected to the liquid reservoir 13 through the outflow pipeline 12 to output the reacted liquid from the reaction system 2. In this embodiment, the microfluidic injection pump assembly 11 is a high-precision injection pump or flow controller, which is used to inject the liquid into the pipeline 12, and the injection flow rate is controlled between 1-200uL / min. In this embodiment, the pipeline 12 is made of corrosion-resistant Teflon material, with an outer diameter of 2mm and an inner diameter of 0.8mm.

[0023] The microfluidic control system 1 further includes electromagnetic on-off valves 14 , which are respectively arranged on the inflow and outflow pipelines 12 to control the on-off of the liquid.

[0024] The microfluidic control system 1 further includes a flow sensor 15 and a pressure sensor 16 , which are respectively disposed on the inflow pipeline 12 to monitor the real-time flux and fluid pressure of the fluid flow.

[0025] The microfluidic control system 1 further includes a controller 17 and a computer 18, wherein the controller 17 is connected to the electromagnetic on-off valve 14, the flow sensor 15 and the pressure sensor 16 through a control line 19 to control the on-off of the electromagnetic valve and read the sensor data as needed, and the computer 18 is connected to the controller 17 to operate and display the controller 17. In this embodiment, the control line 19 communicates via RS485, including an A / B line.

[0026] The reaction system 2 includes an in-situ liquid pool 21 and an electrode 22, wherein the microfluidic control system 1 and the flow channel 211 of the in-situ liquid pool 21 (see Figure 2 ) is connected, the electrode 22 is installed on the in-situ liquid pool 21 and inserted into the flow channel 211 so that the reaction liquid in the flow channel 211 undergoes an electrolytic reaction. In this embodiment, the in-situ liquid pool 21 is made of PEEK (polyetheretherketone), and a part of it is hollowed out and punched to facilitate the pipeline 12 (through such as Figure 2The water inlet and outlet are shown) and the electrode 22 (through Figure 2 The electrode CE, electrode WE, reference electrode) shown in the figure are inserted and installed. In this embodiment, the pipeline 12 uses a 1 / 8 PEEK Luer connector to fix and seal the liquid. In this embodiment, the electrode 22 includes a platinum wire electrode and a reference Ag / AgCl electrode, which are fixedly installed to the in-situ liquid pool 21 using a threaded port.

[0027] The reaction system 2 also includes a silicon nitride window 23 and a rubber sealing O-ring 24, such as Figure 2 and Figure 3 As shown, by fixing the screw 25, the silicon nitride window 23 is pressed to the in-situ liquid pool 21 through the rubber sealing O-ring 24 to achieve sealing. Specifically, in the case of covering the flow channel 211, the silicon nitride window 23 and the rubber sealing O-ring 24 are embedded in the in-situ liquid pool 21, and a thin liquid layer is achieved after being pressed against each other. Among them, the inner diameter of the rubber sealing O-ring 24 is larger than the diameter of the flow channel 211, and the window of the silicon nitride window 23 is located at the center of the rubber sealing O-ring 24. It should be understood that the rubber sealing O-ring 24 has two functions, one is to provide an elastic sealing effect between the in-situ liquid pool 21 and the silicon nitride window 23, and the other is that the liquid in the flow channel 211 enters the inner area of ​​the rubber sealing O-ring 24 to provide a thin liquid layer. Among them, the silicon nitride window 23 is made of silicon nitride film and is used to seal the liquid environment. In this embodiment, the size of the silicon nitride window 23 is 10mm×10mm, and the window in the center is 0.5mm×0.5mm, so that X-rays can pass through to detect the sample. In particular, the thickness of the silicon nitride film is not greater than 200nm, the film stress is <250MPa, and the exit angle at the window is not greater than 45 degrees. The flatness RMS of the silicon nitride window 23 is <1nm, it is resistant to weak acids and weak bases and common organic solvents, and can withstand the negative pressure brought by ultra-high vacuum environment. According to the needs of some experiments, the silicon nitride film can be covered with a metal film or other film as an electrode or substrate. In electrochemical experiments, the silicon nitride window 23 is a silicon nitride window with an electrode.

[0028] The vacuum system 3 includes a vacuum chamber 31, which provides an ultra-high vacuum environment for the in-situ liquid pool 21. In this embodiment, the vacuum chamber 31 is a corrosion-resistant stainless steel processing chamber. It should be understood that how to provide a vacuum environment through the vacuum chamber 31 is a prior art and will not be repeated here.

[0029] For the in-situ liquid pool 21 working in a vacuum-sealed environment, the microfluidic control system 1 provides automatic or semi-automatic liquid sample inlet / outlet. Specifically, the liquid sample is injected into the in-situ liquid pool 21 through the microfluidic injection pump assembly 11, so that the in-situ liquid pool 21 can be replaced. The continuous injection and replacement of the liquid sample can also realize the cleaning and sample replacement functions of the in-situ liquid pool 21. During the in-situ experiment, the liquid maintains continuous flow, and the flow rate is from several to tens of microliters per minute. The gas-related experiments control the pressure (for example, up to several atmospheres), and the controller 17 can monitor the liquid flow in real time. When the flow rate is set to 20μm / min and the running time is set to 600s, Figure 4 The real-time monitoring readings of the flow sensor of the in-situ liquid pool when the microfluidic injection pump is operating normally are shown. When liquid leaks, that is, the readings of the flow sensor 15 and the pressure sensor 16 fluctuate more than twice the stable readings within 2 seconds, the controller 17 will determine that liquid leakage has occurred. At this time, the control program quickly (response time is less than 20ms) closes the electromagnetic on-off valve 14 to prevent the liquid from continuing to flow, and displays an alarm signal on the computer 18. Figure 5 The test results of two flow mutations are shown, namely, the flow sensor detected a sudden abnormal increase in liquid flow, and the solenoid valve was able to respond quickly to the flow mutation and actively close to avoid liquid leakage.

[0030] In summary, according to the in-situ reaction flowing liquid system of the utility model, the in-situ liquid pool 21 suitable for working in an ultra-high vacuum environment can realize timely replacement and replenishment of the liquid, can ensure that the in-situ liquid pool 21 does not leak in the ultra-high vacuum environment during the detection process, and meets the purposes of easy use and good stability.

[0031] The above is only a preferred embodiment of the utility model, and is not intended to limit the scope of the utility model. The above embodiments of the utility model can also be modified in various ways. That is, all simple, equivalent changes and modifications made according to the claims and the contents of the specification of the utility model application fall within the scope of protection of the claims of the utility model patent. The conventional technical contents are not described in detail in the utility model.

Claims

1. An in-situ reaction flowing liquid system, characterized in that: The in-situ reaction flow liquid system includes a microfluidic control system, a reaction system and a vacuum system, wherein the reaction system includes an in-situ liquid pool, the microfluidic control system is connected to the flow channel of the in-situ liquid pool to input flowing reaction liquid into the in-situ liquid pool and output reacted liquid, the in-situ liquid pool is fixedly installed in the vacuum system to provide a vacuum sealing environment for the in-situ liquid pool through the vacuum system, and in the in-situ liquid pool, the liquid is provided in the flow form of a thin sample layer and reacts.

2. The in-situ reaction flowing liquid system according to claim 1, characterized in that: The microfluidic control system includes a microfluidic injection pump component and a liquid storage tank, wherein the microfluidic injection pump component is connected to the in-situ liquid pool through an inflow pipeline to introduce reaction liquid into the in-situ liquid pool, and the in-situ liquid pool is connected to the liquid storage tank through an outflow pipeline to output the reacted liquid from the in-situ liquid pool.

3. The in-situ reaction flowing liquid system according to claim 2, characterized in that: The microfluidic control system also includes electromagnetic on-off valves, which are respectively arranged on the inflow and outflow pipelines to control the on-off of the liquid.

4. The in-situ reaction flowing liquid system according to claim 3, characterized in that: The microfluidic control system further comprises a flow sensor and a pressure sensor, which are respectively arranged on the inflow pipeline to monitor the real-time flux and fluid pressure of the fluid flow.

5. The in-situ reaction flowing liquid system according to claim 4, characterized in that: The microfluidic control system also includes a controller and a computer, wherein the controller is connected to the electromagnetic on-off valve, flow sensor and pressure sensor through control lines to control the on-off of the electromagnetic valve and read sensor data, and the computer is connected to the controller to operate and display the controller.

6. The in-situ reaction flowing liquid system according to claim 1, characterized in that: The reaction system also includes electrodes, which are installed on the in-situ liquid pool and inserted into the flow channel so that the reaction liquid in the flow channel undergoes an electrolytic reaction.

7. The in-situ reaction flowing liquid system according to claim 1, characterized in that: The reaction system also includes a silicon nitride window and a rubber sealing O-ring. The silicon nitride window is pressed to the in-situ liquid pool through the rubber sealing O-ring to achieve sealing.

8. The in-situ reaction flowing liquid system according to claim 7, characterized in that: The silicon nitride window has a window for X-rays to pass through.

9. The in-situ reaction flowing liquid system according to claim 8, characterized in that: The inner diameter of the rubber sealing O-ring is larger than the diameter of the flow channel, and the window is located at the center of the rubber sealing O-ring.

10. The in-situ reaction flowing liquid system according to claim 1, characterized in that: The vacuum system includes a vacuum chamber that provides a vacuum environment for the in-situ liquid pool.

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