Method and system for determining sintering parameters of pellets

Abstract

The embodiments of the present application relate to the technical field of chemical informatics, and specifically to a method and system for determining the sintering parameters of a pellet. In the first aspect, the embodiments of the present application provide a method for determining the sintering parameters of a pellet, and the sintering parameters include a predetermined temperature and a predetermined pressure that need to be reached during the sintering process. In the second aspect, the embodiments of the present application also provide a system for determining the sintering parameters of a pellet, and the system includes: a sample preparation module, a sintering module, a sintering gas supply module, a heating module, an image pickup and processing module, and a processor. Through the method and system of the present application, the correspondence between the predetermined pressure, the predetermined temperature, and the dimensional change of the pellet during the pellet sintering process can be determined, so that the sintering parameters can be determined according to the expected pellet size, so as to accurately control the sintering conditions, reduce the defects and errors in the regulation of the sintering parameters, effectively improve the control ability of the pellet sintering process, and obtain a pellet that meets the expected requirements.

Description

Technical Field

[0001] The embodiments of the present application relate to the technical field of chemical informatics, and more particularly to a method and system for determining sintering parameters of a pellet. Background Art

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

[0003] Pellet sintering refers to the process of sintering raw materials into hard solid blocks under high temperature conditions. In the field of heat storage, pellet sintering can be used to manufacture heat storage material pellets to store heat in the form of high density and high heat capacity.

[0004] In order to obtain pellets that meet expected requirements, it is usually necessary to determine the sintering environment conditions in advance and set the sintering parameters. However, there are still many problems in the existing technology in accurately determining the sintering parameters according to expectations, which affects the practical application of pellet sintering technology. Summary of the Invention

[0005] A brief overview of the present application is provided below 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 key or important portions of the present application, nor is it intended to limit the scope of the present application. Its purpose is simply to present certain concepts in a simplified form as a prelude to the more detailed description that will be discussed later.

[0006] In a first aspect, an embodiment of the present application provides a method for determining sintering parameters of a pellet, wherein the sintering parameters include a predetermined temperature and a predetermined pressure required to be reached during the sintering process. The method comprises the following steps: S10: forming a pellet sample from a pellet raw material and placing the pellet sample in a sintering space; S20: evacuating the sintering space; S30: introducing hydrogen into the sintering space to a predetermined pressure; S40: heating the sintering space to a predetermined temperature and obtaining an image of the raw material during the heating process; S50: processing the image to determine a dimensional change of the pellet sample during the heating process and during the process of heating to the predetermined temperature and maintaining the temperature; S60: varying the predetermined pressure and the predetermined temperature, and repeating steps S30, S40, and S50; S70: obtaining data on a plurality of predetermined pressures, predetermined temperatures, and corresponding dimensional changes of the pellets;

[0007] S80: Determine the corresponding relationship between the predetermined pressure, the predetermined temperature and the size change of the pellet according to the data obtained in step S70; S90: Determine the sintering parameters of the pellet according to the expected pellet size.

[0008] On the second aspect, an embodiment of the present application further provides a system for determining the sintering parameters of a core block, the sintering parameters including a predetermined temperature and a predetermined pressure required to be reached during the sintering process, the system comprising: a sample preparation module, configured to prepare a core block sample from a core block raw material; a sintering module, the sintering module forming a sintering space, the core block sample being fed into the sintering module for testing after sample preparation by the sample preparation module is completed; a sintering gas supply module, the sintering gas supply module being configured to input the required test gas to a predetermined pressure into the sintering space; a heating module, the heating module being configured to heat the sintering space so that it meets the test requirements of sintering; an image pickup and processing module, the image pickup and processing module being configured to pick up an image of the core block sample during the heating process and when heated to a predetermined temperature, and to determine its dimensional change based on the image; a processor, the image pickup and processing module sending the dimensional change data of the core block sample to the processor, the processor determining the correspondence between the predetermined pressure, predetermined temperature and the dimensional change of the core block based on the dimensional change of the core block sample and the predetermined temperature and predetermined pressure, and determining the sintering parameters of the core block based on the expected core block size.

[0009] The method and system in the embodiments of the present application determine the correspondence between the predetermined pressure, the predetermined temperature and the dimensional change of the core block during the sintering process of the core block by obtaining the dimensional change of the core block sample when it is sintered at multiple predetermined pressures and multiple predetermined temperatures in the sintering space. Therefore, in actual application, the sintering parameters can be determined according to the expected core block size, so as to accurately control the sintering conditions, reduce the defects and errors in the regulation of the sintering parameters, effectively improve the control ability of the core block sintering process, and obtain core blocks that meet the expected requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] 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, which will help to provide a comprehensive understanding of the present application.

[0011] Figure 1 is a flow chart of a method for determining sintering parameters of a pellet according to one embodiment of the present application;

[0012] Figure 2 3 is a schematic structural diagram of a system for determining sintering parameters of a pellet according to an embodiment of the present application.

[0013] Description of reference numerals:

[0014] 10. Sintering module; 11. Sintering space; 12. Sample stage; 20. Heating module; 21. Heating element; 22. Temperature control element; 30. Image pickup and processing module.

[0015] 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

[0016] Exemplary embodiments of the present application will be described below with reference to the accompanying drawings. For the sake of clarity and conciseness, not all features of actual implementations 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 depending on the implementation. In addition, it should be understood that although the development work may be very complex and time-consuming, it is a routine task for those skilled in the art who benefit from the content of this application.

[0017] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, the accompanying drawings only show the device structure and / or processing steps that are closely related to the solution according to the present application, while other details that are not closely related to the present application are omitted.

[0018] The inventors of this application have discovered that the sintering process of the core blocks usually needs to be carried out in a complex sintering environment, and the key parameters of the sintering environment have an important influence on the size of the sintered core blocks. For example, improper temperature control of the sintering space can easily affect the shrinkage, hardness and surface morphology of the core blocks, and improper pressure control of the sintering space can affect the density of the core blocks. However, there is currently no method that can determine the sintering parameters that match the expected core block size, so that the obtained core blocks can better meet the expected requirements.

[0019] Based on this, an embodiment of the present application provides a method for determining the sintering parameters of a pellet, wherein the sintering parameters include a predetermined temperature and a predetermined pressure required to be reached during the sintering process, such as Figure 1 As shown, Figure 1 A flow chart showing a method for determining sintering parameters of a pellet according to an embodiment of the present application is provided. The method includes the following steps S10 to S90:

[0020] S10: preparing a pellet sample from the pellet raw material, and placing the pellet sample into a sintering space.

[0021] S20: Evacuate the sintering space.

[0022] S30: hydrogen is introduced into the sintering space to a predetermined pressure.

[0023] S40: heating the sintering space to a predetermined temperature, and obtaining an image of the shape of the core block sample during the heating process.

[0024] S50: Processing the appearance image to determine the dimensional change of the core block sample during the heating process and the process of heating to a predetermined temperature and maintaining the temperature.

[0025] S60: Changing the predetermined pressure and the predetermined temperature, and repeating steps S30, S40, and S50.

[0026] S70: Obtain data on a plurality of predetermined pressures, predetermined temperatures, and corresponding changes in pellet size.

[0027] S80: Determine the corresponding relationship between the predetermined pressure, the predetermined temperature and the size change of the pellet according to the data obtained in step S70.

[0028] S90: Determine the sintering parameters of the pellets according to the expected pellet size.

[0029] The method provided in the embodiments of the present application determines the correspondence between the predetermined pressure, the predetermined temperature and the dimensional change of the core block during the sintering process of the core block by obtaining the dimensional change of the core block sample when it is sintered at multiple predetermined pressures and multiple predetermined temperatures in the sintering space. Therefore, in actual application, the sintering parameters can be determined according to the expected core block size, so as to accurately control the sintering conditions, reduce the defects and errors in the regulation of the sintering parameters, effectively improve the control ability of the core block sintering process, and obtain a core block that meets the expected requirements.

[0030] In some embodiments, in step S10, the core block raw material is used to prepare a core block sample in a glove box. After the preparation is completed, the core block sample is placed in a sintering space under the condition of isolating oxygen, so that the process of preparing the core block sample and transferring the core block sample is isolated from oxygen, preventing the core block sample from being oxidized and the generated oxides from affecting the sintering process, thereby affecting the size of the sintered core blocks.

[0031] In some embodiments, in step S20, argon gas is first input to clean the sintering space, and then the pellet sample is placed, and then the sintering space is vacuumed to prevent the pellet sample from being oxidized in the sintering space and avoid affecting the subsequent sintering process.

[0032] Specifically, in step S20, a vacuum replacement method can be adopted. First, the sintering space is vacuumed, and then argon is introduced into it. Then the sintering space is vacuumed again, and then argon is introduced into it. The above steps are repeated 2-3 times to completely replace the oxygen inside the sintering space to ensure the cleaning effect of the sintering space.

[0033] In step S30 , slightly positive pressure hydrogen may be first input into the sintering space to a predetermined pressure to ensure that the pressure in the sintering space remains stable. For example, the predetermined pressure may be set to 0.15 MPa.

[0034] In step S40, after the sintering space is heated to a predetermined temperature, for example, 1700°C, the sintering space is kept at the predetermined temperature for a predetermined time, for example, 3 hours, to ensure that the reaction of the pellet sample is complete, to increase the density of the pellet, and to promote the molding of the pellet.

[0035] Furthermore, in step S40, when acquiring the appearance image of the core block sample, appearance images of multiple core block samples may be acquired during the process of heating the sintering space to a predetermined temperature and during the heat preservation process, so as to determine the dimensional change of the core block sample.

[0036] In some embodiments, in step S40, when the sintering space is heated to a predetermined temperature, the pressure of the sintering space is adjusted to be less than the predetermined pressure, so as to promote the reaction and accelerate the sintering process.

[0037] For example, when the predetermined temperature is 1700°C and the predetermined pressure is 0.15 MPa, in step S40, when the sintering space is heated to 1700°C, the pressure of the sintering space can be adjusted from 0.15 MPa to 0.1 MPa to accelerate the sintering process of the core block sample and facilitate obtaining its appearance image.

[0038] In some embodiments, in step S40, when the heating temperature reaches 800°C, the sintering space is evacuated, and then hydrogen is introduced to clean the sintering space, and then heating is continued to intervene in the sintering process of the pellets to prevent volatiles generated by sintering from affecting the observation of the pellet state.

[0039] Specifically, in step S40, when the heating temperature reaches 800°C, the sintering space is evacuated, and then hydrogen is introduced to a predetermined pressure. The sintering space is then evacuated, and then hydrogen is introduced again. The above steps are repeated 2-3 times to fully remove the volatiles in the sintering space, so as to obtain a clear image of the core block sample later, which is conducive to observing the core block size.

[0040] In some embodiments, when the sample is sintered, the standard sample is also sintered at the same time. According to the size change of the standard sample after sintering, the size acquisition equipment used in step S40 is calibrated to eliminate the deviation of the size data of the core block sample collected by the size acquisition equipment and obtain accurate core block sample size data.

[0041] Among them, the sintering parameters and sintering process of the standard sample are kept completely consistent with those of the core block sample to ensure the accuracy and reliability of the calibration.

[0042] In some embodiments, step S50 further includes the following steps:

[0043] S51: Preprocessing the obtained multiple shape images to obtain contour features of each shape image.

[0044] S52: Determine the size of the core block corresponding to each shape image according to the contour features of each shape image.

[0045] S53: Determine the size change of the core block according to the size of the core block corresponding to each shape image.

[0046] In this embodiment, the contour features of each shape image obtained during the sintering process are extracted, and the core block size corresponding to the image is determined based on the contour features to facilitate quantification of the core block size, thereby more intuitively reflecting the size change of the core block and improving the accuracy of the obtained core block size change data.

[0047] In some embodiments, in step S51, the method further includes:

[0048] S511: De-noising and enhancing the multiple shape images.

[0049] S512: Segment the processed multiple shape images according to their features.

[0050] S513: Extracting contour features of the shape image from the segmented region.

[0051] In this embodiment, multiple shape images are subjected to denoising and enhancement processing to remove random noise and interference in the images and improve image quality. The processed images are then segmented to separate the core blocks from the background, thereby facilitating the extraction of contour features of the shape images from the segmented regions and improving the accuracy of the core block size determined based on the contour features.

[0052] In step S80, a plurality of predetermined pressures, predetermined temperatures, and corresponding changes in the size of the core blocks can be fitted based on the data obtained in step S70 to obtain a relationship curve reflecting the corresponding relationship between the predetermined pressures, predetermined temperatures, and the changes in the size of the core blocks; a relationship between the predetermined pressures, predetermined temperatures, and the changes in the size of the core blocks can be determined based on the relationship curve, and whether the goodness of fit of the relationship curve meets predetermined requirements can be judged based on the relationship curve; and the fitting method can be optimized and adjusted based on the judgment result to determine a new relationship curve, thereby improving the accuracy of the corresponding relationship between the determined predetermined pressures, predetermined temperatures, and the changes in the size of the core blocks.

[0053] The embodiment of the present application also provides a system for determining the sintering parameters of the pellet, wherein the sintering parameters include a predetermined temperature and a predetermined pressure required to be reached during the sintering process, such as Figure 2 As shown, Figure 2A schematic diagram of a system for determining sintering parameters of a pellet according to an embodiment of the present application is shown. The system includes: a sample preparation module configured to prepare pellet samples from pellet raw materials; a sintering module 10, wherein the sintering module 10 is formed with a sintering space 11, into which the pellet samples are fed for testing after being prepared by the sample preparation module; a sintering gas supply module configured to supply required test gas to a predetermined pressure into the sintering space 11; a heating module 20, wherein the heating module 20 is configured to heat the sintering space 11 to meet sintering test requirements; an image pickup and processing module 30, wherein the image pickup and processing module 30 is configured to capture an image of the pellet sample during the heating process and when heated to a predetermined temperature, and to determine a dimensional change thereof based on the image; and a processor, wherein the image pickup and processing module 30 sends dimensional change data of the pellet sample to the processor. The processor determines a correspondence between the predetermined pressure, the predetermined temperature, and the dimensional change of the pellet based on the dimensional change of the pellet sample, the predetermined temperature, and the predetermined pressure, and determines the sintering parameters of the pellet based on the expected pellet size.

[0054] By using the system provided in the embodiments of the present application, it is possible to obtain the dimensional changes of the core block sample when it is sintered at multiple predetermined pressures and multiple predetermined temperatures in the sintering space 11, and determine the correspondence between the predetermined pressure, predetermined temperature and the dimensional change of the core block during the sintering process of the core block. Therefore, in actual application, the sintering parameters can be determined according to the expected core block size, so as to accurately control the sintering conditions, reduce the defects and errors in the regulation of the sintering parameters, effectively improve the control ability of the core block sintering process, and obtain core blocks that meet the expected requirements.

[0055] In some embodiments, the sintering module 10 further includes a sample stage 12 , which is disposed inside the sintering space 11 . After the pellet sample is prepared by the sample preparation module, it is transferred to the sample stage 12 for a sintering test.

[0056] In some embodiments, the heating module 20 includes multiple heating elements 21 and a temperature control element 22. The multiple heating elements 21 are arranged around the sample stage 12 to ensure that the core block samples placed on the sample stage 12 are heated evenly; the temperature control element 22 is configured to measure the temperature of the sintering space 11 and control the heating element 21 to stop heating when the sintering space 11 reaches a predetermined temperature, so as to accurately control the sintering temperature and improve the test accuracy.

[0057] In some embodiments, the sample preparation module is set in the glove box and the process of sending the core block sample from the sample preparation module to the sintering module 10 is also completed in the glove box, so that the sample preparation and transfer of the core block sample are isolated from oxygen, preventing the core block sample from being oxidized and the generated oxides from affecting the sintering process, thereby affecting the size of the sintered core block.

[0058] The process of determining the sintering parameters of the pellets in this application is further explained below with reference to specific examples.

[0059] In a glove box, the core block raw material is made into a core block sample, and the core block sample is placed in a sintering space under the condition of isolating oxygen; a vacuum replacement method is adopted to first vacuum the sintering space, and then argon is introduced into it, and then the sintering space is vacuumed and argon is introduced again, and the above steps are repeated 2-3 times to clean the sintering space, and then the core block sample is placed, and then the sintering space is vacuumed; slightly positive pressure hydrogen is introduced into the sintering space to 0.15MPa; the sintering space is heated, and when the heating temperature reaches 800℃, the sintering space is vacuumed, and then hydrogen is introduced to a predetermined pressure, and then the sintering space is vacuumed. The sintering space is then heated to 1700°C and then the pressure in the sintering space is adjusted to 0.1 MPa, and the temperature is kept at this temperature for 3 hours. The shape images of multiple core block samples are obtained during the heating process to 1700°C and the temperature is kept at this temperature for 3 hours. The obtained shape images are subjected to denoising and enhancement processing. According to the features of the processed images, the regions are segmented, and the contour features of the shape images are extracted from the segmented regions. According to the contour features of each shape image, the contour features of each shape image are determined. The method comprises the steps of: determining the size of the pellet corresponding to the shape image, and determining the dimensional change of the pellet sample during the heating process and the process of heating to a predetermined temperature and maintaining the temperature constant based on the size of the pellet corresponding to each shape image; changing the predetermined pressure and the predetermined temperature, repeatedly injecting hydrogen into the sintering space, heating the sintering space, and obtaining the shape image of the pellet sample, and determining the dimensional change of the pellet sample; obtaining data of a plurality of predetermined pressures, predetermined temperatures, and the corresponding dimensional changes of the pellet; fitting the plurality of predetermined pressures, predetermined temperatures, and the corresponding dimensional changes of the pellet based on the obtained data to obtain a relationship curve reflecting the corresponding relationship between the predetermined pressures, predetermined temperatures, and the dimensional changes of the pellet; determining a relationship between the predetermined pressures, predetermined temperatures, and the dimensional changes of the pellet based on the relationship curve, and judging whether the goodness of fit of the relationship curve meets a predetermined requirement based on the relationship curve; and optimizing and adjusting the fitting method based on the judgment result to determine a new relationship curve, thereby obtaining the corresponding relationship between the predetermined pressures, predetermined temperatures, and the dimensional changes of the pellet; and determining the sintering parameters of the pellet based on the determined corresponding relationship between the predetermined pressures, predetermined temperatures, and the dimensional changes of the pellet based on the expected pellet size.

[0060] 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.

[0061] 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 determining sintering parameters of a pellet, wherein the sintering parameters include a predetermined temperature and a predetermined pressure to be achieved during the sintering process, characterized in that: It includes the following steps: S10: preparing a pellet sample from the pellet raw material, and placing the pellet sample into a sintering space; S20: evacuating the sintering space; S30: Introducing hydrogen into the sintering space to a predetermined pressure; S40: heating the sintering space to a predetermined temperature, and obtaining an image of the shape of the core block sample during the heating process; S50: processing the appearance image to determine the dimensional change of the core block sample during the heating process and the process of heating to a predetermined temperature and maintaining the temperature; S60: changing the predetermined pressure and the predetermined temperature, and repeating steps S30, S40, and S50; S70: Obtaining data on a plurality of predetermined pressures, predetermined temperatures, and corresponding changes in pellet size; S80: Determine the corresponding relationship between the predetermined pressure, the predetermined temperature and the size change of the pellet according to the data obtained in step S70; S90: Determine the sintering parameters of the pellets according to the expected pellet size.

2. The method according to claim 1, characterized in that In step S10, the pellet raw material is used to prepare the pellet sample in a glove box. After the preparation is completed, the pellet sample is placed in the sintering space under the condition of isolating oxygen.

3. The method according to claim 1, characterized in that In step S20, argon gas is first input to clean the sintering space, and then the core block sample is placed therein, and then the sintering space is vacuumed.

4. The method according to claim 1, wherein In step S40 , when the sintering space is heated to a predetermined temperature, the pressure of the sintering space is adjusted to be lower than the predetermined pressure.

5. The method according to claim 1, wherein In step S40, when the heating temperature reaches 800°C, the sintering space is evacuated, and then hydrogen is introduced to clean the sintering space, and then heating is continued.

6. The method according to claim 1, characterized in that When the sample is sintered, the standard sample is also sintered at the same time. According to the size change of the standard sample after sintering, the size collection device used in step S40 is calibrated.

7. The method according to claim 1, characterized in that In step S50, the following steps are also included: S51: Preprocessing the obtained multiple shape images to obtain contour features of each shape image; S52: determining the size of the core block corresponding to each shape image according to the contour features of each shape image; S53: Determine the size change of the core block according to the size of the core block corresponding to each shape image.

8. The method according to claim 7, characterized in that In step S51, the following steps are also included: S511: performing denoising and enhancement processing on the multiple appearance images; S512: Segmenting the processed multiple appearance images according to their features; S513: Extracting contour features of the outline image from the segmented region.

9. A system for determining sintering parameters of a pellet, wherein the sintering parameters include a predetermined temperature and a predetermined pressure to be achieved during the sintering process, characterized in that: It includes: a sample preparation module configured to prepare a pellet sample from the pellet raw material; A sintering module is formed with a sintering space, and the pellet sample is sent into the sintering module for testing after being prepared by the sample preparation module; a sintering gas supply module, the sintering gas supply module being configured to input required test gas into the sintering space to a predetermined pressure; a heating module, configured to heat the sintering space to meet sintering test requirements; an image pickup and processing module configured to pick up images of the core block sample during the heating process and when heated to a predetermined temperature and to determine a dimensional change thereof based on the images; The image pickup and processing module sends the dimensional change data of the core block sample to the processor, and the processor determines the corresponding relationship between the predetermined pressure, predetermined temperature and the dimensional change of the core block based on the dimensional change of the core block sample and the predetermined temperature and predetermined pressure, and determines the sintering parameters of the core block based on the expected core block size.

10. The system according to claim 9, characterized in that The sample preparation module is arranged in a glove box, and the process of transferring the pellet sample from the sample preparation module to the sintering module is also completed in the glove box.

Images