In-situ high-temperature Raman testing device suitable for four-column press

Abstract

The invention belongs to the field of material performance testing, and particularly relates to an in-situ high-temperature Raman testing device suitable for a four-column press, the in-situ high-temperature Raman testing device comprises an upper cover, a device main body and the four-column press, the upper cover is provided with a Raman window, the device main body is provided with a storage cavity, and the upper cover covers the device main body to form a sealing cavity; an air inlet clamping sleeve connector and an air outlet flange connector are formed in the side face of the device body, the four-column press is arranged in the middle of the device body, sleeve components of the four-column press are of hollow structures, and a sample containing mechanism, a heating furnace and a thermocouple are arranged in the four-column press. The sample placing mechanism is arranged in the center of the four-column press, a sample is positioned in the sample placing mechanism, the heating furnace is arranged around the sample, and the thermocouple is arranged on the side of the sample. The heating furnace is used for performing multi-temperature-section heating on the sample, and the Raman spectrum analysis of the sample under the high-temperature and high-pressure conditions can be realized in cooperation with a corresponding Raman device.

Description

Technical Field

[0001] The invention belongs to the field of material performance testing, and in particular relates to an in-situ high-temperature Raman testing device suitable for a four-column press. Background Art

[0002] Raman spectroscopy is based on the Raman scattering effect. By analyzing the scattered spectrum with different frequencies from the incident light, information on molecular vibration and rotation is obtained, thereby further obtaining detailed information such as the chemical structure, crystallinity and molecular interactions of the sample. This Raman spectroscopy is widely used in many fields such as chemistry, physics, biology, materials science, and earth sciences. It has important value in qualitative analysis, highly quantitative analysis, and molecular structure determination. However, due to technical limitations, Raman spectroscopy is mainly used under experimental conditions of normal temperature and pressure. A few technical means can measure the Raman spectrum of materials under normal pressure and high temperature conditions, but the measurement means of materials under high temperature and high pressure conditions are still relatively scarce, which is not conducive to exploring the Raman spectrum characteristics of materials under high temperature and high pressure conditions.

[0003] Therefore, how to provide an in-situ high-temperature Raman testing device suitable for a four-column press has become a problem that those skilled in the art need to consider. Summary of the invention

[0004] In view of the problems existing in the above-mentioned prior art, the present invention discloses an in-situ high-temperature Raman testing device suitable for a four-column press. The present invention combines a four-column press with a heating furnace to produce the high-temperature and high-pressure conditions required for the in-situ Raman test, greatly expanding the temperature and pressure range of the in-situ Raman test, thereby exploring the Raman spectral characteristics of the material under high-temperature and high-pressure conditions. The present invention specifically discloses the following technical solutions:

[0005] An in-situ high-temperature Raman testing device suitable for a four-column press comprises an upper cover, a device body and a four-column press, wherein the upper cover is provided with a Raman window, the device body is provided with a storage cavity, the upper cover is mounted on the device body to form a sealed cavity, the side of the device body is provided with an air inlet ferrule interface and an air outlet flange interface, the four-column press is arranged in the middle of the device body, the sleeve components of the four-column press are all hollow structures, a sample placement mechanism, a heating furnace and a thermocouple are arranged inside the four-column press, the sample placement mechanism is arranged at the center of the four-column press, the sample is located in the sample placement mechanism, the heating furnace is arranged around the sample, and the thermocouple passes through the heating furnace and is arranged on the side close to the sample.

[0006] Furthermore, the sample placement mechanism includes a tungsten carbide pad, an upper diamond anvil, a lower diamond anvil and a sample cavity. The tungsten carbide pad is matched with a sleeve component and is provided with a conical hole. The upper diamond anvil and the lower diamond anvil are respectively bonded to the tungsten carbide pad. The sample cavity is arranged between the upper diamond anvil and the lower diamond anvil. A sample chamber is arranged in the middle of the sample cavity.

[0007] Furthermore, the base of the four-column press is provided with an air circuit interface, which can be connected to an air inlet ferrule interface. The bottom of the base near the lower diamond anvil is provided with an air inlet hole, and an inert atmosphere is introduced to prevent the lower diamond anvil and the upper diamond anvil from oxidizing at high temperature.

[0008] Furthermore, the heating furnace is installed on the lower base of the four-column press through a gasket, and the heating furnace is arranged in a ring shape.

[0009] Furthermore, it also includes a water cooling system, which includes a water cooling interlayer, a water cooling interface and an external water cooling circulation machine. The water cooling interlayer is arranged in the device body and the upper cover, and the water cooling interface is arranged on the outer surface of the device body and the upper cover, and is connected to the external water cooling circulation machine to form an overall water circuit circulation.

[0010] Furthermore, a line expansion interface and a thermocouple power supply interface are also provided on the surface of the device body.

[0011] Furthermore, a power adapter block and a thermocouple adapter block are provided inside the device body. The power adapter block is electrically connected to the heating furnace and the line expansion interface respectively, and the thermocouple adapter block is electrically connected to the thermocouple and the thermocouple power interface respectively.

[0012] Furthermore, the Raman window includes a Raman light window and a quartz window plate. The Raman light window is arranged at the center of the upper cover. The diameter of the Raman light window is 15 mm. The quartz window plate covers the surface of the Raman light window.

[0013] The beneficial effects of the present invention are:

[0014] 1. The invention can provide the required high-pressure environment for sample testing through the setting of the four-column press. After the heating furnace is powered on, it can provide environmental field heating for the sample, so that the sample can be heated up, and the maximum temperature can reach above 1000°C. The setting of the thermocouple, in conjunction with the external temperature controller, can accurately control the heating temperature, so that the temperature control accuracy is maintained at ±1°C, and the physical phase structure of the sample under high temperature and high pressure environment can be studied. It is a powerful auxiliary means in many research fields such as materials science and earth science;

[0015] 2. The present invention provides an air inlet ferrule interface and an air outlet flange interface, so that nitrogen, argon or a small amount of hydrogen can be introduced into the sealed cavity formed by the device body and the upper cover as a protective gas, thereby protecting the four-column press. The present invention provides an air path interface and an air inlet hole on the four-column press, so that the protective gas can flow evenly through the surface of the diamond anvil first, thereby avoiding oxidation of the diamond anvil at high temperature. After the gas is fully in contact with the diamond anvil, it can be quickly discharged through the radiation through hole provided in the heating furnace, thereby avoiding gas retention. The gas is recovered after being discharged from the device;

[0016] 3. The present invention is connected to an external water-cooling machine circulation machine through a water-cooling interface, so as to continuously absorb and conduct away the overflowed heat, thereby ensuring the safety of the experimental process. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the main structure of the present invention;

[0018] Figure 2 It is a schematic diagram of the internal structure of the main body of the device of the present invention;

[0019] Figure 3 It is a cross-sectional view of the upper cover of the present invention;

[0020] Figure 4 It is a front view of the four-column press of the present invention;

[0021] Figure 5 A top view of the four-column press of the present invention;

[0022] Figure 6 for Figure 5 Sectional view of the middle AA plane;

[0023] Figure 7 for Figure 6 A partial enlarged schematic diagram in the middle;

[0024] Figure 8 This is a schematic diagram of the cooperation between the heating furnace and the tungsten carbide pad of the present invention;

[0025] Fig. 9 It is a schematic diagram of the structure of the heating furnace of the present invention.

[0026] Among them, 1. upper cover; 2. device body; 3. four-column press; 4. quartz window; 5. air inlet ferrule interface; 6. air outlet flange interface; 7. hollow cavity; 8. heating furnace; 9. thermocouple; 10. round gasket; 11. thermocouple bracket; 12. line expansion interface; 13. thermocouple power interface; 14. power adapter block; 15. thermocouple adapter block; 16. tungsten carbide pad; 17. upper diamond anvil; 18. lower diamond anvil; 19. sample cavity; 21. sample chamber; 22. gas path interface; 23. air inlet; 24. through hole; 25. water-cooling interlayer; 26. water-cooling interface. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] Example 1

[0029] Refer to the attached Figure 1-9 This embodiment discloses an in-situ high-temperature Raman test device suitable for a four-column press, including an upper cover 1, a device body 2 and a four-column press 3. The device body 2 and the upper cover 1 in this embodiment are both made of hard 316L stainless steel or other hard metal materials. A Raman light window with a diameter of 15 mm is arranged at the center of the upper cover 1, which is covered by a quartz window plate 4 as a Raman window, allowing the Raman beam to pass through, performing in-situ Raman spectrum analysis on the sample, and playing a certain sealing and protective role. The device body 2 is provided with a storage cavity to provide a placement space for all components. The upper cover 1 is installed on the device body 2 and fits tightly to form a sealed cavity. The four-column press 3 is arranged in the middle of the device body 2 to provide the high-pressure environment required for the in-situ test. The side of the device body 2 is provided with an air inlet ferrule interface 5 and an air outlet flange interface 6, which can be introduced with nitrogen, argon or a small amount of hydrogen as a protective gas, thereby protecting the four-column press 3 and reducing the influence of high temperature on it.

[0030] The sleeve parts of the four-column press 3 in the present invention are respectively provided with hollow cavities 7, and the interior of the four-column press 3 is provided with a sample placement mechanism, a heating furnace 8 and a thermocouple 9 facing the hollow cavity 7. The sample placement mechanism is arranged at the center of the four-column press 3, and the sample is located in the sample placement mechanism for the pressurization experiment of the sample. The heating furnace 8 is arranged around the sample. Specifically, the heating furnace 8 is arranged in a ring shape, and the heating furnace 8 is installed on the lower base of the four-column press 3 through a circular gasket 10. The heating furnace 8 of the present invention is made of platinum to provide a stable high-temperature environment for the sample, and the temperature can reach above 1000°C. The thermocouple 9 is arranged on the side close to the sample through an electric couple bracket 11 and through the heating furnace 8 to obtain the temperature of the sample. According to experimental requirements, the present invention can adopt thermocouples 9 of types K, B, S, etc., and an external temperature controller with a temperature control accuracy of ±1°C. The temperature of the sample is obtained in real time and fed back to the temperature control terminal immediately. The temperature control terminal analyzes the data and outputs a signal to control the speed regulation module to regulate the output current of the heating furnace 8. This set of processes can be combined with the program control software and displayed in real time on the software interface.

[0031] In order to realize the testing of samples, the surface of the device body 2 is also provided with a line extension interface 12 and a thermocouple power supply interface 13. The line extension interface 12 is used to connect an external power supply and a temperature controller, and the thermocouple power supply interface 13 is used to connect a thermocouple power supply. The inside of the device body 2 is provided with a power adapter block 14 and a thermocouple adapter block 15. The power adapter block 14 is electrically connected to the heating furnace 8 and the line extension interface 12 respectively, and the thermocouple adapter block 15 is electrically connected to the thermocouple 9 and the thermocouple power supply interface 13 respectively.

[0032] The sample placement mechanism of the present invention comprises a tungsten carbide pad 16, an upper diamond anvil 17, a lower diamond anvil 18 and a sample cavity 19, wherein the upper diamond anvil 17 and the lower diamond anvil 18 are respectively bonded to the tungsten carbide pad 16, the sample cavity 19 is arranged between the upper diamond anvil 17 and the lower diamond anvil 18, and a sample chamber 21 is arranged in the middle of the sample cavity 19 for placing the sample.

[0033] As a preferred embodiment of the present invention, the lower base of the four-column press 3 is provided with an air circuit interface 22, which is connected to the air inlet ferrule interface 5. An air inlet hole 23 is provided at the bottom of the base near the lower diamond anvil 18. The protective gas enters through the air inlet ferrule interface 5, and after being discharged from the air inlet hole 23, it will preferentially flow evenly over the surface of the diamond anvil to avoid oxidation of the upper diamond anvil 17 and the lower diamond anvil 18 at high temperature. After filling the device body 2, the protective gas is discharged from the air outlet flange interface 6 for recovery.

[0034] As a preferred embodiment of the present invention, in order to prevent gas from being trapped and to achieve rapid exhaust, the heating furnace 8 is provided with through holes 24 in a radial shape.

[0035] As a preferred embodiment of the present invention, the present invention also includes a water cooling system, which includes a water cooling interlayer 25, a water cooling interface 26 and an external water cooling circulation machine. The water cooling interlayer 25 is arranged in the device body 2 and the upper cover 1, and the water cooling interface 26 is arranged on the outer surface of the device body 2 and the upper cover 1. It is connected to the external water cooling machine circulation machine through the water cooling interface 26 to form an overall water circuit circulation, which continuously absorbs and conducts away the overflowed heat, thereby ensuring the safety of the experimental process.

[0036] The above description is only a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any slight modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. An in-situ high temperature Raman testing device suitable for a four-column press, characterized in that: It includes an upper cover, a device body and a four-column press, the upper cover is provided with a Raman window, the device body is provided with a storage cavity, the upper cover is installed on the device body to form a sealed cavity, the side of the device body is provided with an air inlet ferrule interface and an air outlet flange interface, the four-column press is arranged in the middle of the device body, the sleeve parts of the four-column press are all hollow structures, the inside of the four-column press is provided with a sample placement mechanism, a heating furnace and a thermocouple, the sample placement mechanism is arranged at the center of the four-column press, the sample is located in the sample placement mechanism, the heating furnace is arranged around the sample, and the thermocouple passes through the heating furnace and is arranged on the side close to the sample.

2. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 1, characterized in that: The sample placement mechanism includes a tungsten carbide pad, an upper diamond anvil, a lower diamond anvil and a sample cavity. The tungsten carbide pad is matched with a sleeve component and is provided with a conical hole. The upper diamond anvil and the lower diamond anvil are respectively bonded to the tungsten carbide pad. The sample cavity is arranged between the upper diamond anvil and the lower diamond anvil. A sample chamber is arranged in the middle of the sample cavity.

3. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 2, characterized in that: The sleeve component of the four-column press is provided with an air circuit interface, which can be connected to an air inlet ferrule interface. The sleeve component is provided with an air inlet hole near the bottom of the lower diamond anvil, and an inert atmosphere is introduced to prevent the lower diamond anvil and the upper diamond anvil from oxidizing at high temperature.

4. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 1, characterized in that: The heating furnace is installed on the sleeve component of the four-column press through a gasket, and the heating furnace is arranged in a ring shape.

5. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 1, characterized in that: It also includes a water cooling system, which includes a water cooling interlayer, a water cooling interface and an external water cooling circulation machine. The water cooling interlayer is arranged in the device body and the upper cover, and the water cooling interface is arranged on the outer surface of the device body and the upper cover, and is connected to the external water cooling circulation machine to form an overall water circuit circulation.

6. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 1, characterized in that: The surface of the device body is also provided with a line expansion interface and a thermocouple power supply interface.

7. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 6, characterized in that: A power adapter block and a thermocouple adapter block are arranged inside the device body. The power adapter block is electrically connected to the heating furnace and the line expansion interface respectively, and the thermocouple adapter block is electrically connected to the thermocouple and the thermocouple power interface respectively.

8. The in-situ high temperature Raman testing device suitable for a four-column press according to claim 1, characterized in that: The Raman window comprises a Raman light window and a quartz window plate. The Raman light window is arranged at the center of the upper cover. The diameter of the Raman light window is 15 mm. The quartz window plate covers the surface of the Raman light window.

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