Device for measuring high-temperature wettability of fused salt and electrode material

Abstract

The utility model discloses a device for measuring the high-temperature wettability of fused salt and an electrode material. The device comprises a furnace body, the furnace body is provided with an internal containing cavity, an opening is formed in the side face of the furnace body, an air inlet is formed in the lower portion of the furnace body, and an air outlet is formed in the upper portion of the furnace body; the object placing table is arranged in the internal accommodating cavity and is used for placing fused salt and an electrode material; the furnace cover is connected to the opening in an openable and closable mode, a window is arranged on the furnace cover, and the position of the window is matched with the position of the storage table; the measuring assembly is matched with the window and is used for shooting and measuring the wetting angle of the fused salt and the electrode material; the heating sleeve sleeves the furnace body and is used for heating the furnace body; the induction temperature adjusting assembly is matched with the heating sleeve and used for adjusting the heating temperature of the heating sleeve; the gas supply assembly is connected with the gas inlet and used for conveying argon into the inner containing cavity. According to the device disclosed by the embodiment of the utility model, the fused salt and the electrode material can be measured in a high-temperature and high-pressure environment.

Description

Technical Field

[0001] The utility model belongs to the technical field of electrochemical metallurgy, and in particular relates to a device for measuring the high-temperature wettability of molten salt and electrode materials. Background Art

[0002] In the field of electrochemical metallurgy, the use of molten salt electrolysis to refine rare refractory metals is a common and efficient method. High-temperature molten salt can easily penetrate into the microstructure under pressure, affecting the progress of the reaction and the purity of the product. Therefore, it is necessary to study the wetting of molten salt and electrode materials; however, the existing contact angle tester cannot expose the sample to high temperature and high pressure. Utility Model Content

[0003] In view of this, some embodiments disclose a device for measuring high-temperature wettability of molten salt and electrode material, comprising:

[0004] The furnace body has an internal cavity, an opening is formed on the side of the furnace body, an air inlet is formed at the bottom of the furnace body, and an air outlet is formed at the top of the furnace body;

[0005] A storage table is arranged in the internal cavity and is used to place molten salt and electrode materials;

[0006] The furnace cover is connected to the opening in an openable and closable manner, and a viewing window is provided on the furnace cover, and the position of the viewing window is adapted to the position of the storage table;

[0007] A measuring component, adapted to the viewing window, for photographing and measuring the wetting angle between the molten salt and the electrode material;

[0008] A heating sleeve is mounted on the furnace body and is used to heat the furnace body;

[0009] An induction temperature adjustment component is matched with the heating sleeve and is used to adjust the heating temperature of the heating sleeve;

[0010] The gas supply component is connected to the gas inlet and is used to transport argon gas into the internal cavity.

[0011] Some embodiments disclose a device for measuring high-temperature wettability of molten salt and electrode materials, wherein a solenoid valve is provided in the gas outlet.

[0012] In some embodiments, the device for measuring the high-temperature wettability of molten salt and electrode material disclosed herein, the induction temperature adjustment component includes:

[0013] A power regulator is electrically connected to the heating sleeve and is used to adjust the heating power of the heating sleeve;

[0014] The temperature sensor is adapted to be arranged in the internal cavity of the furnace body, is electrically connected to the power regulator, and is used to detect the actual temperature in the internal cavity.

[0015] Some embodiments disclose a device for measuring the high-temperature wettability of molten salt and electrode materials, which also includes a heat-insulating sleeve, which is arranged on the heating sleeve and is used to insulate the furnace body.

[0016] Some embodiments disclose a device for measuring the high-temperature wettability of molten salt and electrode materials, which further includes an outer shell, which is sleeved in a heat-insulating sleeve.

[0017] In the device for measuring the high-temperature wettability of molten salt and electrode materials disclosed in some embodiments, a sealing ring is provided on the furnace cover.

[0018] Some embodiments disclose a device for measuring high-temperature wettability of molten salt and electrode materials, wherein the furnace body is a cylindrical structure.

[0019] Some embodiments disclose a device for measuring high-temperature wettability of molten salt and electrode material, wherein the measuring component comprises:

[0020] A camera is used to capture the wetting process of the molten salt and the electrode material;

[0021] The image processor is electrically connected to the camera and is used to measure and analyze the wetting angle between the molten salt and the electrode material.

[0022] In the device for measuring the high-temperature wettability of molten salt and electrode materials disclosed in some embodiments, a pressure sensor is also provided in the internal cavity of the furnace body.

[0023] In some embodiments, the device for measuring the high-temperature wettability of molten salt and electrode material disclosed herein comprises a storage platform comprising:

[0024] A support frame is fixedly arranged in the internal cavity of the furnace body;

[0025] A receiving box is detachably arranged on the supporting frame, and the receiving box has a top opening;

[0026] The storage plate is detachably covered on the top opening of the receiving box, and the storage plate is a mesh structure.

[0027] The device for measuring the high-temperature wettability of molten salt and electrode materials disclosed in the embodiment of the utility model is simple and reliable to operate, has high measurement accuracy, and can place molten salt and electrode materials in a high-temperature and high-pressure environment for measurement. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 Example 1 is a schematic diagram of the structure of an apparatus for measuring the high-temperature wettability of molten salt and electrode materials.

[0029] Reference numerals

[0030] 1 Stove body 2 Storage table

[0031] 3 Temperature sensor 4 Furnace cover

[0032] 5 Window 6 Measurement components

[0033] 7 Heating jacket 8 Insulation jacket

[0034] 9 Outer shell 10 Air supply assembly

[0035] 11 Power Regulator 101 Air Inlet

[0036] 102 Air outlet DETAILED DESCRIPTION

[0037] The word "embodiment" used here as an "exemplary" does not necessarily mean that any embodiment described is superior to or better than other embodiments. Unless otherwise specified, the performance index tests in the embodiments of this application are performed using conventional test methods in the art. It should be understood that the terms described in this application are only used to describe specific implementation methods and are not used to limit the content disclosed in this application.

[0038] Unless otherwise specified, the technical and scientific terms used in this document have the same meanings as commonly understood by ordinary technicians in the technical field to which this application belongs; other experimental methods and technical means not specifically specified in this application refer to experimental methods and technical means commonly used by ordinary technicians in this field.

[0039] The terms "substantially" and "approximately" used herein are used to describe small fluctuations. For example, they can refer to less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. The numerical data represented or presented in the range format herein are used only for convenience and brevity, and should therefore be flexibly interpreted as including not only the values ​​clearly listed as the limits of the range, but also all independent values ​​or sub-ranges contained in the range. For example, the numerical range of "1-5%" should be interpreted as including not only the clearly listed values ​​of 1% to 5%, but also the independent values ​​and sub-ranges within the range shown. Therefore, independent values ​​such as 2%, 3.5% and 4% and sub-ranges such as 1%-3%, 2%-4% and 3%-5% are included in this numerical range. This principle also applies to the range of only one numerical value. In addition, such an interpretation applies regardless of the width of the range or the characteristics described.

[0040] In this document, including in the claims, transitional words such as "comprises," "includes," "with," "having," "containing," "involving," "accommodating," etc. are understood to be open-ended, i.e., meaning "including but not limited to." Only the transitional words "consisting of" and "composed of" are closed transitional words.

[0041] In order to better illustrate the content of the present application, numerous specific details are provided in the specific examples below. It should be understood by those skilled in the art that the present application can also be implemented without certain specific details. In the embodiments, some methods, means, instruments, equipment, etc. well known to those skilled in the art are not described in detail in order to highlight the main purpose of the present application.

[0042] Under the premise of no conflict, the technical features disclosed in the embodiments of the present application can be arbitrarily combined, and the obtained technical solutions belong to the contents disclosed in the embodiments of the present application. It should be noted that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like mentioned in the present application indicate the orientation or position relationship based on the orientation or position relationship shown in the accompanying drawings, which is only for the convenience of describing the technical features 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 understood as a limitation of the present invention, unless it conflicts with the context. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance, unless it conflicts with the context.

[0043] In some embodiments, the apparatus for measuring high temperature wettability of molten salt and electrode material comprises:

[0044] The furnace body has an internal cavity, an opening is provided on the side of the furnace body, an air inlet is provided at the bottom of the furnace body, and an air outlet is provided at the top of the furnace body; generally, the air inlet and the air outlet are located on the diagonal line of the furnace body so that the argon gas entering the furnace body can fill the entire furnace body;

[0045] A storage table is arranged in the internal cavity and is used to place molten salt and electrode materials;

[0046] The furnace cover is connected to the opening in an openable and closable manner, and a viewing window is arranged on the furnace cover, and the setting position of the viewing window is adapted to the setting position of the storage platform; generally, when molten salt and electrode materials are arranged on the storage platform, the focus point of the measuring component, the center point of the viewing window, and the contact surface of the molten salt and the electrode material are located on the same axis, and the measuring component can take a clear picture of the wetting process of the molten salt and the electrode material;

[0047] A measuring component, adapted to the viewing window, for photographing and measuring the wetting angle between the molten salt and the electrode material;

[0048] A heating sleeve is mounted on the furnace body and is used to heat the furnace body;

[0049] An induction temperature adjustment component is matched with the heating sleeve and is used to adjust the heating temperature of the heating sleeve;

[0050] The gas supply component is connected to the gas inlet and is used to transport argon gas into the internal cavity.

[0051] In some embodiments, a solenoid valve is disposed in the gas outlet.

[0052] In some embodiments, a pressure sensor is also provided in the internal cavity of the furnace body. Generally, the pressure sensor detects the argon gas pressure in the furnace body so that the furnace body reaches a suitable pressure; when the pressure in the furnace body is too high, the solenoid valve in the gas outlet will automatically open to release the pressure.

[0053] In some embodiments, the induction temperature adjustment component includes:

[0054] A power regulator is electrically connected to the heating sleeve and is used to adjust the heating power of the heating sleeve;

[0055] The temperature sensor is adapted to be arranged in the internal cavity of the furnace body, is electrically connected to the power regulator, and is used to detect the actual temperature in the internal cavity. As an optional embodiment, the temperature sensor is a thermocouple.

[0056] Generally, the power regulator adjusts the heating power of the heating jacket in real time according to the actual temperature detected by the temperature sensor, so that the temperature of the furnace body can be maintained at the set temperature when measuring the wettability of the molten salt and the electrode material.

[0057] In some embodiments, a heat insulating sleeve is further included, which is arranged on the heating sleeve and is used to insulate the furnace body.

[0058] In some embodiments, the device further comprises an outer shell, which is sleeved in the heat-insulating sleeve. Generally, the outer shell is made of metal.

[0059] In some embodiments, a sealing ring is provided on the furnace cover.

[0060] In some embodiments, the furnace body is a cylindrical structure.

[0061] In some embodiments, the measuring component comprises:

[0062] A camera is used to capture the wetting process of the molten salt and the electrode material. Generally, the camera lens is a high-precision telephoto lens that can capture a clear outline image of the molten salt in a high-temperature molten state.

[0063] The image processor is electrically connected to the camera and is used to measure and analyze the wetting angle between the molten salt and the electrode material. Generally, the image processor is provided with ImageJ software to process and analyze the captured images, and the ImageJ software can measure the wetting angle between the molten salt and the electrode material at various time points.

[0064] Generally, the measurement methods of high-temperature wettability of molten salt and electrode materials include:

[0065] The electrode material is set to a block sample with a length and width of 5 to 10 mm and a height of 3 to 5 mm and is placed on a storage table;

[0066] 1-3 g of molten salt is pressed at 1-7 MPa for 2-6 min to form a molten salt block, which is placed on the electrode material;

[0067] Close the furnace cover, seal the furnace body, and deliver argon gas into the furnace body through the air inlet;

[0068] After the argon gas fills the cavity, open the solenoid valve in the gas outlet and adjust the flow rate of the argon gas so that the argon gas can bulge out evenly and slowly in the form of bubbles;

[0069] The furnace body is heated to the set temperature through the heating jacket and the induction temperature control component;

[0070] The wetting process of the molten salt and the electrode material is photographed by a camera at a speed of 0.1 to 1 second per frame, and the photographed images are processed using ImageJ software to measure the wetting angle between the molten salt and the electrode material.

[0071] In some embodiments, the storage platform includes:

[0072] A support frame is fixedly arranged in the internal cavity of the furnace body;

[0073] A receiving box is detachably arranged on the supporting frame, and the receiving box has a top opening;

[0074] The storage plate is detachably covered on the top opening of the receiving box, and the storage plate is a mesh structure.

[0075] Generally, the molten salt block will melt into a flowing state at high temperature. If the wettability of the molten salt and the electrode material is low, the molten salt will flow downward along the electrode material to the storage table, and even flow into the internal cavity of the furnace body, causing pollution to the storage table and the internal cavity of the furnace body; therefore, in this embodiment, the storage table is configured as a detachable structure of a support frame, a receiving box and a storage plate. During the measurement process, the molten salt in a flowing state flows from the storage plate with a mesh structure to the receiving box and is collected by the receiving box. After the measurement, the storage plate and the receiving box can be disassembled for cleaning, so that the device for measuring the high-temperature wettability of molten salt and electrode materials disclosed in the embodiment of the utility model can be reused.

[0076] In some embodiments, the furnace body is a cylindrical stainless steel chamber.

[0077] In some embodiments, the storage table is made of stainless steel.

[0078] In some embodiments, the window is made of high temperature resistant quartz glass.

[0079] The technical details are further illustrated below in conjunction with embodiments.

[0080] Example 1

[0081] Figure 1 This is a schematic diagram of the structure of the device disclosed in Example 1 for measuring the high-temperature wettability of molten salt and electrode materials.

[0082] like Figure 1 As shown, the device for measuring the high-temperature wettability of molten salt and electrode material includes a furnace body 1, an opening is provided at the left end of the furnace body 1, an air inlet 101 is provided at the lower left part of the furnace body 1, and an air outlet 102 is provided at the upper right part of the furnace body 1. A storage table 2 and a temperature sensor 3 are arranged inside the furnace body 1, and the temperature sensor 3 is located below the storage table 2. A furnace cover 4 is arranged on the opening of the furnace body 1, and a window 5 is adapted to be arranged on the furnace cover 4. A measuring component 6 is arranged at a position opposite to the left side of the window 5, a heating sleeve 7 is provided on the outside of the furnace body 1, and an insulating sleeve 8 is provided on the outside of the heating sleeve 7, and an outer shell 9 is provided on the outside of the insulating sleeve 8, and an air supply component 10 and a power regulator 11 located on the right side of the air supply component 10 are arranged below the furnace body 1, and the air supply component 10 is connected to the air inlet 101, and the power regulator 11 is electrically connected to the temperature sensor 3 and the heating sleeve 7.

[0083] Example 2

[0084] This embodiment discloses a method for measuring the high-temperature wettability of NaCl molten salt and graphite, and the specific steps are as follows:

[0085] Take 1-3g NaCl molten salt for briquetting;

[0086] Place graphite on a storage table in the internal cavity of the furnace body, and place a NaCl molten salt block on the graphite;

[0087] Close the furnace cover, seal the furnace body, and deliver argon gas into the furnace body through the air inlet;

[0088] After the argon gas fills the cavity, open the solenoid valve in the gas outlet and adjust the flow rate of the argon gas so that the argon gas can bulge out evenly and slowly in the form of bubbles;

[0089] Heat the furnace body to 750℃ through the heating jacket and induction temperature control assembly and keep it warm for 30 minutes;

[0090] The wetting process of NaCl molten salt and graphite was photographed by a camera at a speed of 0.1 to 1 second per frame, and the captured images were measured using ImageJ software. It was found that the wetting angle of NaCl molten salt to graphite was maintained at about 120°, and the wetting angle of NaCl molten salt to graphite was almost unchanged. It can be seen that the wetting ability of NaCl molten salt to graphite is poor.

[0091] Example 3

[0092] This embodiment discloses the NaCl-KCl molten salt and ZrC x O y The measurement method of high temperature wettability is as follows:

[0093] Take 1-3g NaCl-KCl molten salt for briquetting;

[0094] ZrC x O y Place the NaCl-KCl molten salt block on the ZrC x O y superior;

[0095] Close the furnace cover, seal the furnace body, and deliver argon gas into the furnace body through the air inlet;

[0096] After the argon gas fills the cavity, open the solenoid valve in the gas outlet and adjust the flow rate of the argon gas so that the argon gas can bulge out evenly and slowly in the form of bubbles;

[0097] Heat the furnace body to 750℃ through the heating jacket and induction temperature control assembly and keep it warm for 30 minutes;

[0098] The wetting process of NaCl molten salt and graphite was photographed by a camera at a speed of 0.1 to 1 second per frame, and the captured images were measured using ImageJ software. It was found that the NaCl-KCl molten salt dissolved into ZrC within 1 minute. x O y It can be seen that NaCl-KCl molten salt has a great influence on ZrC x O y Has good wettability.

[0099] The device for measuring the high-temperature wettability of molten salt and electrode materials disclosed in the embodiment of the utility model is simple and reliable to operate, has high measurement accuracy, and can place molten salt and electrode materials in a high-temperature and high-pressure environment for measurement.

[0100] The technical solutions disclosed in the present utility model and the technical details disclosed in the embodiments are merely illustrative of the inventive concept of the present utility model and do not constitute a limitation on the technical solutions of the present utility model. Any conventional changes, replacements or combinations of the technical details disclosed in the embodiments of the present utility model have the same inventive concept as the present utility model and are within the protection scope of the claims of the present utility model.

Claims

1. A device for measuring the high-temperature wettability of molten salt and electrode materials, characterized in that: include: A furnace body, wherein the furnace body has an internal cavity, an opening is formed on the side of the furnace body, an air inlet is formed at the bottom of the furnace body, and an air outlet is formed at the top of the furnace body; A storage table, arranged in the internal cavity, for placing molten salt and electrode materials; A furnace cover, which is openably connected to the opening, and is provided with a viewing window, the position of which matches the position of the storage table; A measuring component, adapted to the window, for photographing and measuring the wetting angle between the molten salt and the electrode material; A heating sleeve, which is sleeved on the furnace body and is used to heat the furnace body; An induction temperature adjustment component, adapted to the heating sleeve and used to adjust the heating temperature of the heating sleeve; A gas supply assembly is arranged to be connected to the gas inlet and is used to deliver argon gas into the internal cavity.

2. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: A solenoid valve is arranged in the air outlet.

3. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: The induction temperature adjustment component comprises: a power regulator, electrically connected to the heating sleeve, and used to adjust the heating power of the heating sleeve; The temperature sensor is adapted to be arranged in the internal cavity of the furnace body, is electrically connected to the power regulator, and is used to detect the actual temperature in the internal cavity.

4. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: It also includes a heat insulation sleeve, which is arranged on the heating sleeve and is used for heat insulation and heat preservation of the furnace body.

5. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 4, characterized in that: It also includes an outer shell, which is sleeved on the thermal insulation sleeve.

6. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: A sealing ring is sleeved on the furnace cover.

7. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: The furnace body is a cylindrical structure.

8. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: The measuring assembly comprises: A camera, used for photographing the wetting process of the molten salt and the electrode material; An image processor is electrically connected to the camera and is used to measure and analyze the wetting angle between the molten salt and the electrode material.

9. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: A pressure sensor is also arranged in the internal cavity of the furnace body.

10. The device for measuring high-temperature wettability of molten salt and electrode material according to claim 1, characterized in that: The storage platform comprises: A support frame, fixedly disposed in the internal cavity of the furnace body; A receiving box is detachably arranged on the supporting frame, and the receiving box has a top opening; The storage plate is detachably covered on the top opening of the receiving box, and the storage plate is a mesh structure.

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