Method for preparing cerium sample and method for converting cerium sample into oxide

Abstract

The embodiment of the invention relates to the technical field of preparation or treatment of rare earth metals, in particular to a method for preparing a cerium sample and a method for converting the cerium sample into an oxide, and the method for preparing the cerium sample comprises the following steps: S1, melting a cerium material; s2, the melt obtained in the step S1 is subjected to ingot casting forming; s3, segmenting the formed object obtained in the step S2; s4, storing the segmentation object obtained in the step S3 in a first organic solvent; s5, removing surface oxides from the segmented object in a first organic solvent; s6, taking out the product obtained in the step S5 from the first organic solvent, and removing the first organic solvent on the surface of the product by using a second organic solvent; s7, removing the second organic solvent on the surface of the product; and S8, determining that the second organic solvent is completely removed. According to the method, oxides on the surface of the cerium can be removed on the premise of avoiding combustion of the cerium, the impurity content in the finally obtained cerium sample is reduced to the maximum extent, and the purity of the cerium sample is effectively improved, so that the subsequent experiment precision is ensured.

Description

Technical Field

[0001] The embodiments of the present application relate to the technical field of preparation or processing of rare earth metals, and specifically to a method for preparing a cerium sample and a method for converting the cerium sample into oxides. Background Art

[0002] The statements herein merely provide background information related to the present application and do not necessarily constitute prior art.

[0003] As a rare earth metal, cerium is widely used in nuclear energy, aerospace and other fields due to its good chemical stability and high corrosion resistance. Cerium metal has good plasticity and ductility. When preparing cerium samples, hot processing, cold processing and chemical processing can be used. However, the current traditional cerium sample preparation method still has problems such as low purity of the prepared cerium samples and contains more impurities. Summary of the invention

[0004] A brief overview of the present application is provided below in order to provide a basic understanding of certain aspects of the present application. It should be understood that this overview is not an exhaustive overview of the present application. It is not intended to identify the key or important parts of the present application, nor is it intended to limit the scope of the present application. Its purpose is merely to present certain concepts in a simplified form as a prelude to a more detailed description discussed later.

[0005] In a first aspect, an embodiment of the present application provides a method for preparing a cerium sample, the method comprising the following steps: S1: melting cerium material; S2: forming an ingot from the melt obtained in step S1; S3: dividing the formed product obtained in step S2; S4: storing the divided product obtained in step S3 in a first organic solvent; S5: removing surface oxides from the divided product in the first organic solvent; S6: taking the product obtained in step S5 out of the first organic solvent, and removing the first organic solvent from the surface of the product using a second organic solvent; S7: removing the second organic solvent from the surface of the product; S8: ensuring that the second organic solvent is completely removed.

[0006] In a second aspect, an embodiment of the present application provides a method for converting a cerium sample into an oxide, wherein the method uses a cerium sample obtained by the method of any embodiment of the first aspect of the present application, and converts the cerium sample into an oxide.

[0007] The method in the embodiments of the present application is to store the obtained split products by melt-casting and splitting the cerium material in a first organic solvent, and treat the split products in the first organic solvent to remove the oxides on the surface of the split products while isolating the split products from the air to prevent them from burning; then, use a second organic solvent to remove the first organic solvent on the surface of the product, and completely remove the second organic solvent to minimize the impurity content in the finally obtained cerium sample, effectively improve the purity of the cerium sample, and thus ensure the accuracy of subsequent experiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Other objects and advantages of the present application will become apparent from the following description of the embodiments of the present application with reference to the accompanying drawings, and will help to provide a comprehensive understanding of the present application.

[0009] Figure 1 The figure is a flow chart of a method for preparing a cerium sample according to one embodiment of the present application.

[0010] Figure 2 The present invention is a flowchart of a method for converting a sample of cerium (Ce) into oxide according to one embodiment of the present application.

[0011] Figure 3 It is a schematic diagram of the structure of a test device according to an embodiment of the present application.

[0012] Figure 4 It is a schematic diagram of the structure of a heating component and a monitoring component according to an embodiment of the present application.

[0013] Figure 5 It is a structural schematic diagram of a test device from another perspective according to an embodiment of the present application.

[0014] Description of reference numerals:

[0015] 10. Shell; 20. Weighing assembly; 21. Weighing piece; 22. Weighing shell; 23. Guide piece; 24. Sealing piece; 25. Gas passage; 26. Support rod; 30. Sample holder; 40. Heating assembly; 401. First space; 402. Second space; 41. Heating shell; 411. Monitoring window; 42. Heating piece; 43. First reaction wall; 44. Second reaction wall; 45. Air inlet passage; 46. Air outlet passage; 47. Support piece; 50. Drive assembly; 51. Drive piece; 52. Drive assembly support piece; 60. Lifting assembly; 61. First-stage lifting piece; 62. Second-stage lifting piece; 63. Third-stage lifting piece; 64. Connecting piece; 70. Monitoring piece; 80. Support frame.

[0016] It should be noted that the drawings are not necessarily drawn to scale, but are merely shown in a schematic manner that does not affect the reader's understanding. DETAILED DESCRIPTION

[0017] Exemplary embodiments of the present application will be described below in conjunction with the accompanying drawings. For the sake of clarity and conciseness, not all features of the actual implementation are described in the specification. However, it should be understood that many implementation-specific decisions must be made in the process of developing any such actual implementation in order to achieve the developer's specific goals, such as meeting those constraints related to the system and business, and these constraints may vary from implementation to implementation. In addition, it should be understood that although the development work may be very complex and time-consuming, it is only a routine task for those skilled in the art who benefit from the content of this application.

[0018] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, only the device structure and / or processing steps closely related to the scheme according to the present application are shown in the accompanying drawings, while other details that are not very relevant to the present application are omitted.

[0019] The inventors of this application discovered that due to the chemical properties of cerium, such as its ability to react with oxygen in the air at room temperature, being extremely susceptible to oxidation and deterioration, and being easy to burn, it is difficult to effectively remove impurities in cerium while ensuring safety during the preparation of cerium samples, thereby increasing the purity of the cerium samples and avoiding affecting the experimental accuracy when used in subsequent experiments.

[0020] Based on this, the embodiment of the present application provides a method for preparing a cerium sample, such as Figure 1 As shown, Figure 1 A flow chart of preparing a cerium sample according to an embodiment of the present application is shown, and the method includes the following steps S1 to S8:

[0021] S1: molten cerium material.

[0022] S2: The melt obtained in step S1 is cast into an ingot.

[0023] S3: Divide the molded product obtained in step S2.

[0024] S4: storing the fraction obtained in step S3 in a first organic solvent.

[0025] S5: removing surface oxides from the partitioned product in the first organic solvent.

[0026] S6: taking out the product obtained in step S5 from the first organic solvent, and removing the first organic solvent on the surface of the product by using a second organic solvent.

[0027] S7: removing the second organic solvent on the surface of the product.

[0028] S8: Determine that the second organic solvent is completely removed.

[0029] The method provided in the embodiments of the present application is to store the obtained split products by melt-casting and splitting the cerium material in a first organic solvent, and treat the split products in the first organic solvent to remove the oxides on the surface of the split products while isolating the split products from the air to prevent them from burning; then, use a second organic solvent to remove the first organic solvent on the surface of the product, and completely remove the second organic solvent to minimize the impurity content in the finally obtained cerium sample, effectively improve the purity of the cerium sample, and thus ensure the accuracy of subsequent experiments.

[0030] In some embodiments, in step S1, the following steps are also included:

[0031] S11: Determine the temperature of the melt in real time.

[0032] S12: Determine the heating power of the melting operation according to the temperature determined in step S11 and the predetermined temperature.

[0033] In this embodiment, the current temperature of the melt is determined in real time and compared with the predetermined temperature to determine the heating power required for the melting operation, thereby facilitating adjustment of the heating power and further removing impurities in the melt.

[0034] In step S12, the predetermined temperature is the temperature at which the cerium material melts and at which the purity of the obtained melt is the highest.

[0035] In step S2, the molten ingot obtained in step S1 may be formed into a cake-like object so as to be subsequently divided into shapes and sizes that meet predetermined requirements.

[0036] In some embodiments, in step S3, the segmentation operation may be performed under an inert gas atmosphere to prevent the molded product obtained in step S2 from reacting with oxygen to generate oxides during the segmentation process.

[0037] For example, dry ice may be used to create an inert gas atmosphere to isolate the molded object from oxygen, while cooling the cutting operation to prevent the molded object from self-igniting.

[0038] In some embodiments, in step S3, the following steps may also be included:

[0039] S31: Cutting the molded product obtained in step S2 into columns of a predetermined size.

[0040] S32: Segment the columnar material obtained in step S31.

[0041] In this embodiment, the formed object obtained in step S2 is cut into columns of a predetermined size, and then the columns are divided into small segments of a predetermined size, so as to obtain a cerium sample that meets the predetermined needs.

[0042] In step S4, after obtaining the partition, the partition is immediately transferred to a first organic solvent for storage to isolate oxygen and prevent the partition from burning. For example, the first organic solvent may be kerosene.

[0043] In step S5, the surface of the partition may be polished with sandpaper in the first organic solvent to remove oxides on the surface of the partition.

[0044] In step S6, the product obtained after removing the surface oxide is taken out from the first organic solvent and placed in a second organic solvent to remove the first organic solvent on the surface of the product. For example, the second organic solvent may be ethanol.

[0045] In some embodiments, in step S7, an inert gas may be used to continuously purge the surface of the product to remove the second organic solvent on the surface of the product, thereby preventing the product from undergoing an oxidation reaction and generating oxides again.

[0046] The second organic solvent is a volatile solvent, which is easy to volatilize when the surface of the product is continuously purged with an inert gas, thereby facilitating complete removal of the second organic solvent and improving the purity of the cerium sample.

[0047] In some embodiments, step S7 may further include the following steps:

[0048] S71: Place the product in a sealed container.

[0049] S72: Evacuate the sealed container.

[0050] S73: Introduce inert gas into the sealed container to purge the product.

[0051] In this embodiment, the product is placed in a sealed container, the air in the sealed container is extracted, and an inert gas is introduced therein, so as to continuously purge the surface of the product with the inert gas, remove the second organic solvent in an environment isolated from oxygen, and avoid oxidation of the product in the process as much as possible.

[0052] Before step S71, before placing the product in a sealed container, the sealed container may be converted into an inert gas atmosphere to prevent the product from being oxidized by the air inside the sealed container when placed in the sealed container.

[0053] In some embodiments, in step S7, the following steps may also be included:

[0054] S74: Collect exhaust gas discharged from the sealed container.

[0055] S75: Determine the composition of the exhaust gas.

[0056] In step S8, it is determined that the second organic solvent is completely removed according to the components of the tail gas determined in step S75.

[0057] In this embodiment, the tail gas discharged from the sealed container is collected and its components are determined to facilitate judgment on whether the second organic solvent is completely removed. The judgment result is highly accurate and effectively avoids residual components of the second organic solvent.

[0058] Specifically, in step S74, while introducing inert gas into the sealed container, the exhaust gas discharged from the sealed container can be continuously collected, and the components of the exhaust gas can be determined in step S75. In step S8, when the exhaust gas components do not contain the second organic solvent, it is determined that the second organic solvent has been completely removed.

[0059] In some embodiments, step S8 may further include the following steps:

[0060] S81: After the product is placed in the sealed container but before the inert gas is introduced, weigh the sealed container.

[0061] S82: In step S73, the sealed container is continuously weighed.

[0062] S83: According to the weighing result in step S82 and the weighing result in step S81, it is determined whether the second organic solvent is completely removed.

[0063] In this embodiment, by comparing the weight of the sealed container before and after the product is purged with the inert gas, it is convenient to efficiently and directly determine whether the second organic solvent is completely removed.

[0064] Specifically, in step S81, after placing the product in a sealed container and evacuating the sealed container, the sealed container is weighed, and then an inert gas is input into the sealed container; in step S82, after inputting the inert gas, the sealed container is continuously weighed to obtain multiple weighing results of the sealed container after inputting the inert gas; in step S83, the multiple weighing results obtained in step S82 are compared with the weighing results in step S81 to obtain multiple comparison results. When the comparison results meet the condition of remaining unchanged within a predetermined time range, it can be determined that the second organic solvent has been completely removed.

[0065] In some embodiments, step S8 may further include the following steps:

[0066] S84: In step S73, the sealed container is continuously weighed.

[0067] S85: According to the weighing result in step S84, it is determined whether the second organic solvent is completely removed.

[0068] In this embodiment, the sealed container is continuously weighed, and the weight change thereof is used to more efficiently and directly determine whether the second organic solvent has been completely removed.

[0069] Specifically, in step S84, after the inert gas is input into the sealed container, the sealed container is continuously weighed to obtain multiple weighing results; in step S85, when it is observed that the multiple weighing results meet the condition of remaining unchanged within a predetermined time range, it can be determined that the second organic solvent has been completely removed.

[0070] In some embodiments, the first organic solvent is soluble in the second organic solvent, so that the second organic solvent can remove the first organic solvent from the surface of the product.

[0071] The cerium sample prepared by the method for preparing a cerium sample provided in the embodiment of the present application can be further converted into oxides, such as Figure 2 As shown, Figure 2 A flow chart showing a method for converting a sample of cerium (Ce) into oxides according to an embodiment of the present application is shown. The method includes the following steps S10 to S60:

[0072] S10: Prepare a sample from cerium (Ce) material.

[0073] S20: placing a sample in a sample holder.

[0074] S30: The driving assembly drives the heating assembly to lower the heating assembly so that the sample holding part can be placed in the heating assembly.

[0075] S40: Inert gas is introduced into the reaction space of the heating component and the reaction space is heated to a predetermined temperature.

[0076] S50: continuously inputting a mixed gas of steam and nitrogen, a mixed gas of steam and argon, or a mixed gas of steam and air into the reaction space.

[0077] S60: Determine that the conversion of the sample into oxides is complete.

[0078] The method provided in the embodiment of the present application is to place a cerium sample in a sample holder, and use a driving component to drive a heating component to be driven downward so that the sample holder can be in the heating component, and then first input an inert gas into the reaction space of the heating component to heat the reaction space, and then continuously input a reaction gas into the reaction space to ensure that the reaction gas can be quickly heated to a predetermined temperature, so that the cerium sample in the sample holder and the reaction gas can fully react, thereby effectively improving the conversion rate of the cerium sample into oxide, ensuring that the cerium sample is completely oxidized, and obtaining a cerium oxide product with stable properties and high purity; and, by determining that the conversion of the sample into oxide is complete, it is convenient to make a clear judgment on the reaction progress, ensuring that the reaction is sufficient and complete, so that the generated cerium oxide product can reach the expected purity.

[0079] In some embodiments, in step S60, the weight of the sample can be determined by a weighing component, and the conversion of the sample into oxides can be determined to be complete based on the weight change of the material.

[0080] In this embodiment, the weight of the material is determined to directly obtain the weight change of the material, thereby accurately and directly determining the reaction progress and judging whether the conversion of the sample into the oxide is complete.

[0081] Specifically, in step S60, the weight of the sample can be monitored in real time using a weighing component. When it is monitored that the weight of the sample remains unchanged or changes very little within a certain period of time, it can be determined that the conversion of the sample into oxides is complete.

[0082] In some embodiments, in step S60, the exhaust gas from the exhaust passage may be collected, and the speed at which the sample is converted into oxides may be determined based on the rate of change of the components of the exhaust gas.

[0083] In this embodiment, the exhaust gas from the exhaust passage is collected to determine the change rate of each component in the exhaust gas compared with the exhaust gas components at the beginning of the reaction. Without affecting the normal reaction process, the speed at which the sample is converted into oxides is determined to judge the current progress of the reaction, thereby determining whether the conversion of the sample into oxides is completed.

[0084] Since in step S50, a mixture of steam and nitrogen, a mixture of steam and argon, or a mixture of steam and air is continuously input into the reaction space as the reaction gas, when the reaction gas undergoes an oxidation reaction with the cerium sample, the conversion rate of the sample into oxide can be determined by detecting the hydrogen concentration in the exhaust gas components.

[0085] Specifically, in step S60, the exhaust gas from the exhaust passage can be collected at the beginning of the reaction to determine the hydrogen concentration in the exhaust gas at this time; and the exhaust gas from the exhaust passage can be collected in real time during the reaction to determine the hydrogen concentration in the exhaust gas components; the hydrogen concentration in the exhaust gas determined in real time during the reaction is compared with the hydrogen concentration in the exhaust gas generated at the beginning of the reaction to determine the rate of change of hydrogen in the exhaust gas from the beginning of the reaction to the current process, so as to determine the speed of conversion of the sample into oxides; and, when the rate of change of hydrogen in the exhaust gas approaches 0 within a certain period of time, it can be determined that the conversion of the sample into oxides is complete.

[0086] In some embodiments, in step S50, the following steps may also be included:

[0087] S51: Superheat the steam before it passes through the reaction space.

[0088] In this embodiment, the steam is superheated so that its temperature exceeds the saturated steam temperature before passing through the reaction space, so that the steam has higher thermal energy, thereby providing a better heating effect, further ensuring that the steam fully reacts with the cerium sample to generate a cerium oxide product with stable properties and high purity.

[0089] In step S50, when a mixture of steam and nitrogen, a mixture of steam and argon, or a mixture of steam and air is continuously input into the reaction space, the input flow rates of steam and nitrogen, argon, or air can be precisely controlled so that the conversion rate can be adjusted in real time according to the current reaction conditions, thereby ensuring that the cerium sample is completely oxidized.

[0090] Among them, when controlling the input flow rate of steam, it can be achieved by controlling the water flow rate input into the container for generating steam. For example, the container for generating steam can be a steam generator, etc. The water input into the steam generator is evaporated through the primary evaporator and continuously heated by the secondary superheater to generate hot steam.

[0091] In some embodiments, in step S50, after the steam enters the reaction space, the steam can first enter a hotter area in the reaction space for preheating, and then enter the reaction area of ​​the reaction space to further increase the steam temperature while ensuring the heating efficiency, thereby ensuring that the cerium sample fully reacts with the steam and effectively improving the conversion rate of the cerium sample into oxides.

[0092] In some embodiments, the method of converting a sample of cerium (Ce) into an oxide may further include the following steps:

[0093] S70: collecting tail gas from the reaction space and cooling the tail gas.

[0094] S80: Inputting the cooled liquid into the container for generating steam in step S50 to generate steam.

[0095] In this embodiment, the tail gas is collected and cooled into liquid, and then the liquid is re-input into the container for generating steam, so as to realize the recycling of the tail gas, improve resource utilization and reduce energy consumption.

[0096] In some embodiments, in step S80, a buffer container may be provided. When the liquid generated in step S70 is too much to be received by the container for generating steam, the liquid is input into the buffer container to avoid overflow caused by excessive liquid in the container for generating steam, thereby affecting the normal generation and input of steam and disrupting the reaction process.

[0097] In some embodiments, in step S50, the relationship between the input mixed gas and the reaction rate can be determined through prior experiments, and the speed or type of the input mixed gas can be determined based on the relationship and the expected reaction rate, so that the type of mixed gas and its input speed that can achieve the expected reaction rate can be selected according to actual reaction needs, thereby facilitating the control and adjustment of the conversion rate of the cerium sample into oxide, ensuring that the cerium sample is completely oxidized, and obtaining a cerium oxide product that meets the expected requirements.

[0098] In some embodiments, the method of converting a sample of cerium (Ce) into oxides in the present application can be implemented using the following experimental device.

[0099] like Figure 3 As shown, Figure 3 The schematic diagram of the structure of the test device of one embodiment of the present application is shown, and the device includes: a housing 10, a weighing assembly 20, a sample holder 30, a heating assembly 40, a driving assembly 50 and a lifting assembly 60. A part of the weighing assembly 20 is arranged in the housing 10, and another part of the weighing assembly 20 is arranged outside the housing 10. The weighing assembly 20 arranged outside the housing 10 is arranged to support the sample holder 30 so as to weigh the sample holder 30; the sample to be processed is arranged in the sample holder 30; the driving assembly 50 is arranged in the housing 10 and is arranged to drive the lifting assembly 60 to move up and down; the lifting assembly 60 is arranged outside the housing 10 and is arranged to drive the heating assembly 40 to move so that the sample holder 30 is inside or outside the heating assembly 40; when the sample holder 30 is arranged inside the heating assembly 40, gas is input into the heating assembly 40 and the heating assembly 40 is heated so that the sample is converted into an oxide.

[0100] The device in this embodiment arranges the heating component 40 to be driven by the lifting component 60 to achieve lifting, so that the reaction gas can be heated in an independent space to ensure that the reaction gas is quickly heated to a predetermined temperature, and the cerium sample in the sample container 30 is located inside the heating component 40 when it needs to be oxidized and fully reacts with the reaction gas, and leaves the heating component 40 after the oxidation is completed, so as to effectively increase the conversion rate of the cerium sample into oxide, ensure that the cerium sample is completely oxidized, and thereby obtain a cerium oxide product with stable properties and high purity.

[0101] like Figure 4 As shown, Figure 4 A schematic structural diagram of a heating component and a monitoring component of an embodiment of the present application is shown. In some embodiments, a first space 401 and a second space 402 are formed in the heating component 40, the heating temperature of the first space 401 is higher than the heating temperature of the second space 402, the gas is configured to first flow into the first space 401, and then flow into the second space 402 after being heated, and the sample holding component 30 is disposed in the second space 402.

[0102] In this embodiment, the heating component 40 is arranged to form a first space 401 and a second space 402, so that the reaction gas is preheated in the first space 401 before flowing into the second space 402, so that the reaction gas is quickly heated to a predetermined temperature before reacting with the cerium sample, thereby ensuring sufficient reaction and complete oxidation of the cerium sample.

[0103] The first space 401 is set to a narrow gap so that the reaction gas can be quickly heated after flowing into the first space 401, and then quickly flow into the second space 402, so as to preheat the reaction gas and increase the reaction gas flow rate, so that it can quickly react with the cerium sample, thereby effectively increasing the conversion rate of the cerium sample into oxides. In addition, the first space 401 can guide the reaction gas, so that the reaction gas moves to the second space 402 along a predetermined flow path.

[0104] In step S50 of the method for converting a cerium (Ce) sample into oxide, steam may be first introduced into the first space 401 through the air intake passage 45 for preheating, and then quickly flow into the second space 402 to react with the cerium sample.

[0105] like Figure 4As shown, in some embodiments, the heating assembly 40 may include: a heating shell 41 , a heating element 42 , a first reaction wall 43 , a second reaction wall 44 , an air inlet passage 45 , an air outlet passage 46 and a support element 47 . The heating shell 41 is configured to be fixedly connected to the lifting assembly 60, and is also configured to be fixedly connected to the support 47. The heating shell 41 and the support 47 form a space, and the heating element 42 is arranged in the space, and the heating element 42 is configured to be fixedly connected to the support 47; the first reaction wall 43 and the second reaction wall 44 are configured to be fixedly connected to the support 47, and the second reaction wall 44 forms a second space 402. The sample holding member 30 can enter the second space 402 for reaction, and a first space 401 is formed between the first reaction wall 43 and the second reaction wall 44; the air inlet passage 45 and the air outlet passage 46 are configured to be fixedly connected to the support 47, and the air inlet of the air inlet passage 45 is arranged in the first space 401, so that the gas is heated by the heating element 42 before entering the second space 402, thereby achieving that the reaction gas is heated to a predetermined temperature before reacting with the cerium sample.

[0106] A predetermined distance is left between the first reaction wall 43 and the second reaction wall 44 , so that the first space 401 is formed into a narrow gap, so that the reaction gas can be quickly heated after flowing into the first space 401 and then quickly flow into the second space 402 .

[0107] The first reaction wall 43 and the second reaction wall 44 are arranged to be sealed and connected to the support member 47, and the air inlet passage 45 and the air outlet passage 46 are arranged to be sealed and connected to the support member 47 to prevent the reaction gas from leaking and affecting the oxidation reaction process, thereby reducing the conversion rate. For example, sealing can be achieved by providing a sealing gland, a sealing ring, etc. at the connection.

[0108] The heating element 42 is arranged between the heating shell 41 and the first reaction wall 43 to heat the reaction gas entering the first space 401 and the second space 402, and the heating element 42 is arranged to have a certain gap with the heating shell 41 to prevent the heating element 42 from directly heating the heating shell 41, thereby causing deformation or damage to the heating shell 41.

[0109] like Figure 3 and Figure 4 As shown, in some embodiments, the test device may further include a monitoring component 70. The heating shell 41 is formed with a monitoring window 411. The monitoring component 70 is arranged outside the heating shell 41. The monitoring window 411 is used to monitor the reaction of the sample in the heating component 40, so as to observe the changes of the sample in real time and determine the reaction progress.

[0110] like Figure 4As shown, in some embodiments, the test device may further include a support frame 80, which is configured to be fixedly connected to the monitoring component 70 and the heating shell 41 to support the monitoring component 70 on the monitoring window 411, so that the monitoring component 70 can monitor the reaction of the sample in the heating component 40 through the monitoring window 411.

[0111] like Figure 5 As shown, Figure 5 A structural schematic diagram showing another perspective of a test device of an embodiment of the present application, in some embodiments, the weighing assembly 20 includes a weighing piece 21, a weighing shell 22, a flow guide 23 and a sealing piece 24. The weighing piece 21 is disposed in the weighing shell 22, the weighing shell 22 is disposed in the shell 10, the flow guide 23 is configured to be fixedly connected with the sealing piece 24, when the sample holding piece 30 enters into the heating assembly 40, the flow guide 23 cooperates with the heating assembly 40 to guide the gas; the sample holding piece 30 is configured to be fixedly connected with the weighing piece 21, the sealing piece 24 is configured to be fixedly connected with the weighing shell 22, when the sample holding piece 30 enters into the heating assembly 40, the flow guide 23 cooperates with the heating assembly 40 to form a seal between the sample holding piece 30 and the heating assembly 40.

[0112] In this embodiment, a guide member 23 is provided to cooperate with the heating assembly 40, so that the reaction gas is guided when the sample holding member 30 enters the heating assembly 40, so as to prevent the high-temperature reaction gas in the heating assembly 40 from flowing into the weighing shell 22, thereby affecting the weighing member 21 and the weighing shell 22, and interfering with the accuracy of the weighing result of the weighing member 21; and a sealing member 24 is provided to be fixedly connected with the guide member 23 and fixedly connected with the weighing shell 22, so as to prevent the reaction gas in the guide member 23 from leaking out.

[0113] like Figure 3 As shown, in some embodiments, the test device may also include a gas passage 25, which is arranged in the weighing shell 22 to input gas into the weighing shell 22 to cool the weighing piece 21 and the weighing shell 22. At the same time, the input gas forms a counter pressure with the reaction gas in the heating component 40 to further prevent the high-temperature reaction gas from flowing into the weighing shell 22.

[0114] For example, inert gas may be introduced into the weighing housing 22 through the gas passage 25 , so that an inert gas atmosphere is formed inside the weighing housing 22 .

[0115] The weighing assembly 20 may further include a support rod 26 , which passes through the guide member 23 and the seal 24 , and one end of the support rod 26 is connected to the sample holding member 30 , and the other end extends into the weighing shell 22 and is connected to the weighing member 21 , so that the weighing member 21 can weigh the sample holding member 30 .

[0116] like Figure 3 As shown, in some embodiments, the driving component 50 includes a driving member 51 and a driving component support member 52, the driving component support member 52 is configured to be fixedly connected to the shell 10, the driving member 51 is configured to be fixedly connected to the driving component support member 52, and the driving member 51 is configured to drive the lifting component 60 to move up and down, so that the lifting component 60 drives the heating component 40 to move.

[0117] In some embodiments, the lifting assembly 60 includes a first-stage lifting member 61, a second-stage lifting member 62 and a third-stage lifting member 63. The driving member 51 drives the first-stage lifting member 61 to move up and down. The first-stage lifting member 61 drives the second-stage lifting member 62 to move up and down. The third-stage lifting member 63 drives the heating assembly 40 to move up and down, thereby making the sample holding member 30 inside or outside the heating assembly 40.

[0118] The first-stage lifting member 61, the second-stage lifting member 62 and the third-stage lifting member 63 can be arranged as a telescopic structure, that is, the third-stage lifting member 63 can extend or retract the second-stage lifting member 62, and the second-stage lifting member 62 can extend or retract the first-stage lifting member 61, so as to flexibly adjust the lifting height of the lifting assembly 60, thereby driving the heating assembly 40 to be adjusted to the predetermined height required for the test.

[0119] like Figure 3 As shown, in some embodiments, the lifting component 60 may further include a connecting member 64, one end of the connecting member 64 is fixedly connected to the third-stage lifting component 63, and the other end of the connecting member 64 is fixedly connected to the heating component 40, so that when the lifting component 60 moves up and down, it can drive the heating component 40 to move up and down.

[0120] In step S30 of the method for converting a cerium (Ce) sample into oxide, when the driving component 50 drives the heating component 40 , the driving component 50 drives the lifting component 60 to descend, and drives the heating component 40 to descend until the sample holder 30 is inside the heating component 40 .

[0121] The following is a specific example to further illustrate the process of preparing cerium samples using the method in this application.

[0122] The cerium material is melted to obtain a melt, and the temperature of the melt is determined in real time during the melting process, and the temperature is compared with a predetermined temperature to determine the heating power required for the melting operation; the melt is cast into a cake-shaped ingot; the cake-shaped molded product is cut into a column of a predetermined size, and the column is divided into small segments of a predetermined size; the obtained segment is immediately transferred to kerosene for storage; in the kerosene, the surface of the segment is polished with sandpaper to remove oxides on the surface of the segment; the product obtained after removing the surface oxide is taken out from the kerosene, and the kerosene on the surface of the product is removed in ethanol; the sealed container is filled with ethanol and the kerosene on the surface of the product is removed. The atmosphere is changed to an inert gas, the product is taken out from the ethanol, placed in a sealed container, the sealed container is evacuated, and the sealed container is weighed, and then an inert gas is introduced into the container to purge the product to evaporate the ethanol; the sealed container is continuously weighed to obtain a plurality of weighing results, and the plurality of weighing results are compared with the weighing results before the inert gas is introduced to obtain a plurality of comparison results. When the comparison result meets the condition of being constant within a predetermined time range and the exhaust gas components discharged from the sealed container do not contain ethanol, it is determined that the ethanol has been completely removed to obtain a cerium sample.

[0123] Regarding the embodiments of the present application, it should also be noted that, in the absence of conflict, the embodiments of the present application and the features therein can be combined with each other to obtain new embodiments.

[0124] The above are only specific implementation methods of the present application, but the protection scope of the present application is not limited thereto. The protection scope of the present application shall be based on the protection scope of the claims.

Claims

1. A method for preparing a cerium sample, characterized in that: It includes the following steps: S1: molten cerium material; S2: forming an ingot from the melt obtained in step S1; S3: dividing the formed product obtained in step S2; S4: storing the fraction obtained in step S3 in a first organic solvent; S5: removing surface oxides from the partitioned product in the first organic solvent; S6: taking out the product obtained in step S5 from the first organic solvent, and removing the first organic solvent on the surface of the product by using a second organic solvent; S7: removing the second organic solvent from the surface of the product; S8: Determine that the second organic solvent is completely removed.

2. The method according to claim 1, characterized in that In step S7, the surface of the product is continuously purged with an inert gas to remove the second organic solvent on the surface of the product.

3. The method according to claim 2, characterized in that In step S7, the following steps are also included: S71: placing the product in a sealed container; S72: evacuating the sealed container; S73: introducing the inert gas into the sealed container to purge the product.

4. The method according to claim 3, characterized in that In step S8, the following steps are also included: S81: after the product is placed in the sealed container but before the inert gas is introduced, weighing the sealed container; S82: In step S73, continuously weighing the sealed container; S83: According to the weighing result in step S82 and the weighing result in step S81, it is determined whether the second organic solvent is completely removed.

5. The method according to claim 3, characterized in that: In step S8, the following steps are also included: S84: In step S73, continuously weighing the sealed container; S85: According to the weighing result in step S84, it is determined whether the second organic solvent is completely removed.

6. The method according to claim 3, characterized in that In step S7, the following steps are also included: S74: collecting tail gas discharged from the sealed container; S75: Determine the components in the exhaust gas; In step S8, it is determined that the second organic solvent is completely removed according to the components of the tail gas determined in step S75.

7. The method according to claim 1, characterized in that In step S3, the segmentation operation is performed under an inert gas atmosphere.

8. The method according to claim 1, characterized in that: The first organic solvent is soluble in the second organic solvent.

9. The method according to claim 1, characterized in that: In step S3, the following steps are also included: S31: cutting the molded object obtained in step S2 into a columnar object of a predetermined size; S32: Segment the columnar material obtained in step S31.

10. The method according to claim 1, characterized in that In step S1, the following steps are also included: S11: Determine the temperature of the melt in real time; S12: Determine the heating power of the melting operation according to the temperature determined in step S11 and the predetermined temperature.

11. A method for converting a cerium sample into an oxide, characterized in that: The method uses a cerium sample obtained by the method according to any one of claims 1 to 10, and converts the cerium sample into an oxide.

Images