KR100886357B1 - Temperature, gas changeable in-situ cell and the controller for X-ray absorption spectroscopy - Google Patents

Abstract

The present invention is directed to an in - situ cell for an X-ray absorptive spectrometer and a controller thereof capable of directly examining the state of a sample without decomposing the cell under constant temperature, pressure, vacuum, and gas atmosphere. The in-situ cell for X-ray absorption spectrometer includes a rectangular container having a first window and a second window at corresponding positions on the front and rear surfaces, and a gas injection / exhaust unit located at an upper surface thereof; A sample mounting part equipped with a sample and corresponding to the positions of the first window and the second window and including a heating metal and a thermocouple, and a sample injection part including one side of the rectangular container; A cooling device disposed on the upper or lower surface of the rectangular container and having a cooling water injection / discharge unit; And an insulating plate interposed between the cooling device and the rectangular container. And a fixing device unit for fixing the cell.

In-situ cell, X-ray, metal window, controller

Description

Temperature, gas changeable in-situ cell and the controller for X-ray absorption spectroscopy

1 is a perspective view of an in-drilling cell for an X-ray absorbing spectrometer according to an embodiment of the present invention;

2 is a perspective view of a rectangular container of an in-drilling cell for X-ray absorbing spectroscopy according to an embodiment of the present invention;

Figure 3 is a perspective view of a sample injection unit of the in-drilling cell for X-ray absorption spectrometer according to an embodiment of the present invention,

Figure 4 is a side view of the sample injection unit of the in-drilling cell for X-ray absorption spectrometer according to an embodiment of the present invention,

5 is a conceptual diagram illustrating a controller of an in-situ cell for an X-ray absorption spectrometer according to an exemplary embodiment of the present invention.

Explanation of reference numerals for the main parts of the drawing

10; Chiller, 20; Insulation Plate,

30; Square container, 40; Sample injection section,

32; A gas injection / exhaust section 33; First and second windows,

34a, 34b; O-rings, 36, 38; O-Ring,

39; Cooling water injection / discharge unit, 43; Sample compartment,

47; Heating system, 50; Fixture Unit,

100; In-situ cells for X-ray absorption spectroscopy, 200; Coolant circulator,

300; Vacuum pump, 400; Gas conditioner

The present invention relates to an in-situ cell for an X-ray absorption spectrometer and a controller thereof, and more particularly, to fabricate a state of a sample under a constant temperature, pressure, vacuum, and gas atmosphere. An in-drilling cell for an X-ray absorption spectrometer and a controller thereof.

The in-drilling cell for the X-ray absorption spectrometer is mainly used to observe the structure of the sample whose state changes according to the change of temperature and the type of gas introduced, and when the specific gas is introduced at a specific temperature, It plays an important role in understanding the oxidation and reduction characteristics.

In general, light source analyzers such as X-rays are mostly exposed to the atmosphere and can only be measured at room temperature, and thus, they do not reconcile with the expectations of researchers and research institutes who wish to observe the state of the sample under various conditions. . Also, in-situ cells are currently used in a limited number of devices, such as infrared spectrometers, so that in-situ (in-situation) can be used to analyze materials without damaging the sample during or after the process. There is a growing interest in analytical methods.

In order to solve the above problem, the Korean Patent No. 2003-0018805 discloses a high temperature X-ray apparatus for high temperature, but the above technique separates the outer container and the window for sample mounting, and removes the outer container and the window after mounting the sample. There is a hassle that needs to be reassembled using a clamp and a frame, and since the material of the window is a polymer, the window may be damaged by a heating source inside the apparatus.

Therefore, the technical problem to be achieved by the present invention is the in-situ cell for X-ray absorption spectroscopy, which is easy to mount a sample without disassembling the cell and can observe the change of in situ state of a wide range of materials such as catalysts, metals and precision materials. Its purpose is to provide a cell and its controller.

In order to achieve the above technical problem, the X-ray absorption spectrometer for an in-drilling cell includes a rectangular container having a first window and a second window at corresponding positions on the front and rear surfaces, and a gas injection / exhaust unit located at an upper surface thereof; A sample mounting part equipped with a sample and corresponding to the positions of the first window and the second window, the sample mounting part including a heating system and a thermocouple, and a sample injection part constituting one side of the rectangular container; A cooling device disposed on the upper or lower surface of the rectangular container and having a cooling water injection / discharge unit; And an insulating plate interposed between the cooling device and the rectangular container. And a fixing device unit fixing the entire cell.

At this time, the first window or the second window may be made of iridium or aluminum, and the first window or the second window is in close contact with the screw through the O-ring between the rectangular container and the high vacuum and constant gas pressure to reach. To be able. For the same purpose, the junction region of the rectangular container and the sample injection unit is also used by being in close contact with a screw through an O-ring. In addition, the cooling device, the heat insulating plate, it may be provided with a hole penetrating the upper portion of the rectangular container, the hole may be connected to the gas injection and discharge portion. In this case, the gas inlet and outlet may be made of a flexible pipe.

The cooling device may be provided with a cooling water flow path therein, the flow path may be a zigzag type of the letter L or S-shape, it is connected to the cooling water injection and discharge.

In addition, the present invention further provides an in-situ cell controller for X-ray absorption spectrometer, which is connected to the in-situ cell for X-ray absorption spectrometer and includes a gas regulator, a cooling water circulator, and a vacuum pump. The gas regulator includes a solenoid valve for introducing gas into the cell, a flow meter for adjusting the inflow amount, a pressure gauge indicating the pressure of the gas in the cell, and the inside of the cell. It can be made of a vacuum gauge (vacuum gauge) indicating the degree of vacuum.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. The following embodiments are provided as examples to sufficiently convey the spirit of the present invention to those skilled in the art. Accordingly, the present invention is not limited to the embodiments described below and may be embodied in other forms. In the drawings, lengths, thicknesses, and the like of layers and regions may be exaggerated for convenience, and like reference numerals denote like elements throughout the specification.

1 is a perspective view of an in-drilling cell for an X-ray absorption spectrometer according to an embodiment of the present invention.

Referring to the drawings, the in-drilling cell 100 for the X-ray absorption spectrometer according to the embodiment of the present invention includes a rectangular container 30 and a sample injection unit 40 installed inside the rectangular container 30. The cooling device 10 is positioned on an upper surface or a lower surface of the rectangular container 30, and an insulation plate 20 is interposed between the cooling device 10 and the rectangular container 30.

The cooling device 10 includes a cooling water injection / discharge unit 39, and a cooling water flow path connected to the cooling water injection / discharge unit 39 is located inside the cooling device 10. Therefore, the cooling water can be circulated into the cooling device 10. The temperature of the cooling water is usually maintained at 10 ° C or less to set the desired temperature. Therefore, even if the temperature of the sample injection unit 40 is increased, the temperature of the in-situ cell 100 body can be kept constant at all times. In addition, the cooling water flow path may have a zigzag shape of a letter or S shape, and in this case, the cooling water flow path may be designed so as not to overlap with the gas injection / exhaust part.

The insulation plate 20 may be an asbestos plate and may be fixed to the square container 30 by screws. By attaching a heat insulating plate 20 having a predetermined thickness to each outer surface of the rectangular container 30, and attaching the cooling device 10 to the top and bottom of the heat insulating plate 20, the in-drilling cell 10. The heat emitted from the heat sink can be prevented from being transferred directly to the cooling device.

In addition, the insulation plate 20 may be interposed between the fixing unit 50 and the rectangular container 30. The fixing unit 50 fixes the entire cell consisting of the rectangular container 30, the sample injection unit 40, the heat insulating plate 20, the cooling device 10. In addition, the fixing device 50 may be made of an external fixing that can be connected to the cell holder and the holder of the X-ray absorption spectrometer.

2 is a perspective view of a rectangular container of an in-drilling cell for X-ray absorbing spectroscopy according to an embodiment of the present invention.

Referring to FIGS. 1 and 2 simultaneously, the front and rear surfaces of the rectangular container 30 are provided with first and second windows 33 at positions corresponding to each other. The first window or the second window 33 may be made of iridium or aluminum. Therefore, by using a metal having a relatively high melting point as the material of the window, compared to a polymer material such as Kapton or imide, it can be used even at a high temperature of 400 ° C or higher. Since the windows must withstand high vacuum and constant gas pressure, the thickness is preferably 0.5T or more.

The first window or the second window 33 is fixed to the round fixing frame with fixing screws via O-rings 34a and 34b on both sides thereof, and then forms a window assembly. The manufactured window assembly may be fixed to the square container 30 with a fixing screw 37, and in this case, an o-ring 38 may be interposed for sealing between the window assembly and the square container 30. . Therefore, the first window or the second window 33 and the rectangular container 30 can be completely sealed, it is possible to maintain a high vacuum and a stable gas pressure.

In addition, a gas injection / exhaust portion 32 is positioned on an upper surface of the rectangular container 30, and the inflow and outflow of gas into the in-drilling cell 100 and the formation of a vacuum are performed by the gas injection / discharge portion 32. Through). In this case, a hole penetrating the upper portion of the cooling device 10, the heat insulating plate 20, and the rectangular container 30 may be provided, and the hole may be connected to the gas injection / discharge unit 32. Further, the gas injection / exhaust portion 32 may be made of a flexible tube.

In other words, the flexible tube is positioned at the top of the cell, and a 1/4 inch hole is vertically penetrated through the top of the cooling device 10, the heat insulator 20, and the rectangular container 30 in order. It can be taken out to allow gas to enter it, and to allow exhaust to another hole.

3 is a perspective view of a sample injection unit of the in-situ cell for X-ray absorption spectrometer according to an embodiment of the present invention, Figure 4 is a sample injection unit of the in- drilling cell for an X-ray absorption spectrometer according to an embodiment of the present invention Side view.

2 to 4, the sample injection unit 40 is installed inside the rectangular container 30 and constitutes one side of the rectangular container 30. The junction region of the rectangular container 30 and the sample injection portion 40 is fixed by the fixing screws 59, the O-ring 36 may be located in the junction region for a complete sealing.

The sample injection portion 40 is formed of an integrated structure of the front plate 41 and the main plate 48. The front plate 41 constitutes one side of the rectangular container 30, and the main plate 48 includes a sample mounting portion 43, a heating system 47, and a thermocouple.

The sample mounting part 43 is located in parallel with the windows corresponding to the positions of the first window and the second window 33. That is, the sample mounting portion 43 has a circular hole is located in parallel with the place where the X-rays are transmitted, the space for mounting the sample in the form of a pellet or film. In addition, a heating system 47 and a thermocouple are positioned around the sample mounting part 43.

For example, a rod-shaped fitting rod may be inserted into the main plate 48, which may be regarded as the periphery of the sample mounting unit 43, and the thermocouple may be mounted inside the sample injection unit 40. The diameter of the quenching rod may be provided differently depending on the temperature to be reached. In this case, the heat insulating material 20 may prevent the heat of the quenching rod from being excessively lost by the cooling devices 10.

5 is a conceptual diagram illustrating a controller of an in-situ cell for an X-ray absorption spectrometer according to an exemplary embodiment of the present invention.

Referring to the drawings, the controller of the in-situ cell for the X-ray absorption spectrometer is connected to the in-situ cell 100 for the X-ray absorption spectrometer of FIG. 1, and includes a gas regulator 400 and a coolant circulator 200. And a vacuum pump 300. The gas regulator 400 may include solenoid valves 80 for introducing gas into the in-situ cell 100, a flow meter 75 for adjusting an inflow amount, and a gas inside the in-drilling cell 100. A pressure gauge 90 indicating a pressure and a vacuum gauge 95 indicating a degree of vacuum inside the in-drilling cell 100 may be included.

The control method of the in- drilling cell internal environment using the controller is as follows. Gas is introduced through the first solenoid valve 81, and the flow meter 75 controls the inflow of the gas by adjusting the inflow amount of the gas. When the second solenoid valve 82 and the fourth solenoid valve 84 are opened, gas is introduced into the in-drilling cell 100. At this time, the fifth solenoid valve 85 is connected to the exhaust line, and opening the fifth solenoid valve 85 may make a flow system.

To convert the interior of the in-situ cell 100 into a vacuum atmosphere, when the fifth solenoid valve 85 is closed and the third solenoid valve 83 is opened, the gas existing in the in-situ cell 100 is opened. Is exhausted. At this time, the vacuum pump 300 is operated and the vacuum pump 300 may use a general rotary pump. By mounting the pressure gauge 90 between the second solenoid valve 82 and the third solenoid valve 3, the pressure in the in-situ cell 100 may be confirmed. In addition, by installing a vacuum gauge at the end of the third solenoid valve 83, it is possible to check the degree of vacuum inside the in-situ cell. The coolant circulator 200 operates while the measurement is performed to thermally protect the in-drilling cell 100 in the desired measurement environment.

Hereinafter, an in-drilling cell for an X-ray absorption spectrometer and a controller thereof according to the present invention will be described with reference to the following experimental examples, but the following experimental examples are not limited thereto.

Experimental Example 1

The in-situ cell was manufactured by assembling the sample injection unit constituting one side of the rectangular container and the rectangular container having the aluminum window installed at the positions corresponding to each other.

 At this time, the windows were formed of iridium or aluminum metal having a relatively high melting point to be stable even at a high temperature of 400 ° C. or more, and a thickness of 0.5T or more. In addition, asbestos plates are attached to the upper and lower portions of the rectangular container and the sample injection unit assembly, respectively, and a cooling device is attached to the upper or lower portion of each asbestos plate so that the heat emitted from the sample injection unit is directly transferred to the cooling unit. Prevented. On the contrary, by attaching the asbestos plate, it was also possible to prevent the internal temperature of the in-drilling cell from being excessively lost by the cooling device, thereby preventing the temperature from rising.

The sample injection unit was manufactured to be made of a front plate and a body plate, and the front plate constituted the front plate of the rectangular container, and the body plate formed a sample mounting unit to be arranged side by side with the windows of the rectangular container. The junction region between the sample injection portion and the rectangular container of the front plate was able to be completely sealed using a set screw and an O-ring. The body plate, which is the inside of the sample injection unit, was manufactured in a rectangular plate shape with a space for inserting a quenting rod and a thermocouple. The sample mounting part was equipped with a circular window having a diameter of 1 cm to mount the sample in the form of pellet or film so as to be parallel to the windows of the rectangular container where the X-rays were transmitted. It can be fixed. In addition, the bottom of the sample mounting portion was inserted into the tingting rod and thermocouple. The diameter of the tingling rod depends on the desired temperature, but in this experiment was inserted into the coating rod of 0.5cm diameter to give a capacity of 600 ℃.

The cooling water flow path was made inside the cooling device to allow the cooling water to circulate during the experiment at a high temperature.

The inflow and outflow of the gas into the in-drilling cell and the vacuum were made through the gas inlet / outlet, and the tube was positioned above the cell using a flexible tube. Two 1 / 4-inch holes were vertically penetrated through the top of the cooling device, asbestos plate, and the square container, and gas was introduced into one of the holes, and the other hole was used to exhaust the holes. I was.

An in-situ cell controller for automatically controlling the temperature and internal atmosphere of the in-situ cell was manufactured by mounting five solenoid valves, pressure gauges and vacuum gauges. In addition, the vacuum and pressure in the in-situ cell can be digitally confirmed through a monitor on the top of the in-situ cell controller body.

The high temperature X-ray in-drilling cell according to the present invention can observe the state change or structural change of the sample according to the temperature and gas atmosphere inside the cell without disassembling the cell, and can withstand high temperature and high vacuum, even under various gas atmospheres. It has the advantage that can be used from room temperature to 600 ℃ while maintaining a stable gas pressure has the effect of observing the thermal stability and redox characteristics of the sample.

In addition, if the controller of the in-situ cell according to the present invention is equipped, the conditions of temperature and gas atmosphere can be easily adjusted according to the experiment.

Although described above with reference to a preferred embodiment of the present invention, those skilled in the art will be variously modified and changed within the scope of the invention without departing from the spirit and scope of the invention described in the claims below I can understand that you can.

Claims (12)

A rectangular container including a first window and a second window provided at corresponding positions on the front and rear surfaces, and a gas injection / exhaust unit located at an upper surface thereof; A sample is mounted and has a sample mounting portion corresponding to the position of the first window and the second window, and a heating system and a thermocouple positioned around the sample mounting portion. Sample injection unit constituting the side; A cooling apparatus located on the upper or lower surface of the rectangular container and having a cooling water injection / discharge unit; An insulating plate interposed between the cooling device and the rectangular container; And In-drilling cell for X-ray absorption spectrometer comprising a fixing device for fixing the entire cell. The method of claim 1, The first window or the second window is in-drilling cell for X-ray absorption spectrometer, characterized in that made of iridium or aluminum. The method of claim 1, An in-drilling cell for an X-ray absorptive spectrometer comprising an O-ring interposed between the first window or the second window and the rectangular container. The method of claim 1, An in-drilling cell for X-ray absorptive spectrometer, comprising: screws for fixing a junction region of the rectangular container and the sample injection portion; and an O-ring positioned in the junction region. The method of claim 1, In-drilling cell for X-ray absorption spectrometer, characterized in that it comprises a cooling device, a heat insulating plate, and a hole penetrating the upper portion of the rectangular vessel. The method of claim 5, wherein And the hole is connected to the gas injection / exhaust unit. The method of claim 6, And the gas inlet / outlet unit comprises a gas inlet and outlet line formed of a flexible tube. The method of claim 1, The cooling apparatus has a high temperature X-ray in-drilling cell, characterized in that it comprises a cooling water flow path connected to the cooling water injection and discharge. The method of claim 8, The cooling water flow path is an in-drilling cell for X-ray absorption spectrometer, characterized in that it has a zigzag form of the letter L or S-shape. The method of claim 1, The insulation plate is an in-drilling cell for X-ray absorption spectrometer, characterized in that the asbestos plate. A controller of an in-situ cell for an x-ray absorptive spectrometer connected to the in-situ cell for an x-ray absorptive spectrometer of claim 1 and comprising a gas regulator, a coolant circulator and a vacuum pump. The method of claim 11, The gas regulator comprises solenoid valves for introducing gas into the cell, a flow meter for adjusting the inflow amount, a pressure gauge indicating the pressure of the gas inside the cell, and a vacuum gauge indicating the degree of vacuum inside the cell. In-drilling cell controller for X-ray absorption spectroscopy.

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