High flow oxide eutectic high-entropy ceramic powder and method of making
By preparing a eutectic mixture of high-entropy rare-earth aluminate phases with low-entropy phases such as Al2O3 through multi-principal solid solution, the problem of poor flowability of oxide ceramic powder was solved, and the preparation of high-flowability oxide eutectic high-entropy ceramic powder was realized, which is suitable for laser additive manufacturing.
Patent Information
- Application Number
- CN202410695609.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-31
- Publication Date
- 2026-01-27
- Estimated Expiration
- 2044-05-31
AI Technical Summary
Commercially available oxide ceramic powders have small particle sizes and irregular shapes, making them prone to agglomeration and resulting in poor flowability, which prevents them from being used properly in laser additive manufacturing technology.
High-entropy oxide eutectic high-entropy ceramic powder was prepared by uniformly mixing a high-entropy rare-earth aluminate phase with a low-entropy phase such as Al2O3 in a eutectic ratio. The powder's flowability and stability were ensured by wet ball milling, drying, grinding, sieving, and high-temperature sintering.
The prepared oxide eutectic high-entropy ceramic powder has excellent flowability, making it suitable for laser additive manufacturing and ensuring the smoothness and stability of the processing.
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Figure CN118515473B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of ceramic materials and relates to a high-flowability oxide eutectic high-entropy ceramic powder and its preparation method. Background Technology
[0002] In recent years, the rapidly developing high-flexibility laser additive manufacturing technology has broken free from the limitations of traditional melt preparation technologies such as directional solidification, which require specific molds and fixtures. It can process samples with more diverse shapes and sizes, becoming a key technology for breaking through the processing of large-size complex structural samples of high-performance oxide eutectic high-entropy ceramics.
[0003] Laser additive manufacturing technology uses highly fluid ceramic powder particles as raw materials, which are uniformly and stably ejected to process the desired sample. However, commercially available oxide ceramic raw material powders have small particle sizes and irregular shapes. When used as raw materials for laser additive manufacturing, they are prone to agglomeration, resulting in poor flowability and making it impossible to properly process the required sample using laser additive manufacturing technology.
[0004] Therefore, it is necessary to provide a high-flowability multi-phase oxide eutectic high-entropy ceramic powder and its preparation method. By preparing a high-flowability oxide eutectic high-entropy ceramic powder, the oxide eutectic high-entropy ceramic powder can have excellent flowability, thereby providing high-quality processing raw materials for laser additive manufacturing technology. Summary of the Invention
[0005] To overcome the problems in the prior art, this invention proposes a high-flowability oxide eutectic high-entropy ceramic powder and its preparation method. A high-entropy rare-earth aluminate phase with multiple principal components in solid solution is prepared using a suitable method. After being uniformly mixed with low-entropy phases such as Al2O3 in a eutectic ratio, the resulting oxide eutectic high-entropy ceramic powder exhibits excellent flowability and can be uniformly and stably delivered by a laser nozzle. This provides high-quality raw materials for laser additive manufacturing technology, ensuring the smooth and normal operation of the laser additive manufacturing process.
[0006] To achieve the above objectives, the present invention is implemented through the following technical solution:
[0007] This invention provides a method for preparing high-flowability oxide eutectic high-entropy ceramic powder, the method comprising the following steps:
[0008] (1) Preparation of multi-principal element solid solution single-phase high-entropy rare earth aluminate ceramic powder: The initial raw material powder is weighed with a molar ratio of Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3 = 25:3:3:3:3:3 or Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3 = 5:1:1:1:1:1. The initial raw material powder is mixed using wet ball milling technology, dried, and then ground and passed through a 1000-mesh sieve. The mixed powder obtained after sieving is calcined and then passed through a 1000-mesh sieve to obtain multi-principal element solid solution single-phase high-entropy rare earth aluminate ceramic powder for later use. The chemical formula of multi-principal element solid solution single-phase high-entropy rare earth aluminate ceramic powder is denoted as (5RE) depending on the molar ratio of the initial raw material powder. 0.2 )3Al5O 12 or (5RE) 0.2 AlO3.
[0009] (2) Preparation of oxide eutectic high-entropy ceramic samples: according to the molar ratio of Al2O3:(5RE) 0.2 )3Al5O 12 =52:12 or Al2O3:(5RE) 0.2 Weigh alumina powder (AlO3 = 54:46) and the multi-principal solid solution single-phase high-entropy rare earth aluminate ceramic powder prepared in step (1). Weigh the Al2O3 powder and (5RE) powder. 0.2 )3Al5O 12 or (5RE) 0.2 After the AlO3 powder is thoroughly mixed, it is dried, ground, and sieved to obtain binary eutectic high-entropy ceramic powder.
[0010] According to the molar ratio Al2O3:(5RE) 0.2 )3Al5O 12 ZrO2 = 38.3:10.7:19.0 or Al2O3:(5RE) 0.2 AlO3:ZrO2 = 39:38:23. Weigh alumina powder, multi-principal component solid solution single-phase high-entropy rare earth aluminate ceramic powder, and ZrO2 powder. After thoroughly mixing the weighed alumina powder, multi-principal component solid solution single-phase high-entropy rare earth aluminate ceramic powder, and ZrO2 powder, dry, grind, and sieve to obtain ternary eutectic high-entropy ceramic powder.
[0011] Binary eutectic high-entropy ceramic powder or ternary eutectic high-entropy ceramic powder is poured into a stainless steel mold and pressed to obtain a blocky eutectic high-entropy ceramic preform. The blocky eutectic high-entropy ceramic preform is then sintered at high temperature to obtain an alumina-based eutectic high-entropy ceramic sample.
[0012] (3) Preparation of oxide eutectic high-entropy ceramic powder: After crushing and sieving the alumina-based eutectic high-entropy ceramic sample obtained in step (2), collect powder particles with a particle size of 15-75 μm to obtain oxide eutectic high-entropy ceramic powder. For powder particles with a particle size greater than the upper limit, continue to crush and sieve until the particle size meets the requirements. For powder particles with a particle size less than the lower limit, re-press, sinter, crush and sieve until the particle size meets the requirements.
[0013] Preferably, the RE2O3 is a rare earth oxide, wherein RE is a rare earth element, including Sc, Y and lanthanides, and the RE12O3 to RE52O3 are five rare earth oxides with the same crystal structure and ionic radii differing by less than 10%.
[0014] Preferably, in step (1), the particle size of Al2O3 powder and the particle size of rare earth oxide powder are both 1 to 5 μm.
[0015] Preferably, in step (1), the wet ball milling medium is anhydrous ethanol, the wet ball milling speed is 300 r / min, and the ball milling time is 12 h.
[0016] Preferably, in step (1), the drying temperature is 80°C and the holding time is 4 to 6 hours.
[0017] Preferably, the calcination temperature in step (1) is 1400-1600℃ and the calcination time is 5-8h.
[0018] Preferably, in step (1), when the molar ratio is Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3 = 25:3:3:3:3:3, the prepared high-entropy rare-earth aluminate ceramic powder has a garnet structure; when the molar ratio is Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3 = 5:1:1:1:1:1, the prepared high-entropy rare-earth aluminate ceramic powder has a perovskite structure.
[0019] Preferably, in step (2), when the high-entropy rare-earth aluminate ceramic powder has a garnet structure, the molar ratio Al2O3:(5RE) is... 0.2 )3Al5O 12 =52:12, molar ratio Al2O3:(5RE) 0.2 )3Al5O 12 ZrO2 = 38.3:10.7:19.0; When the high-entropy rare-earth aluminate ceramic powder has a perovskite structure, the molar ratio Al2O3:(5RE) is 38.3:10.7:19.0. 0.2 AlO3 = 54:46, molar ratio Al2O3:(5RE) 0.2AlO3:ZrO2 = 39:38:23.
[0020] Preferably, in step (2), the pressure for pressing the blocky eutectic high-entropy ceramic preform is 80-120 MPa, and the holding time is 3-5 min.
[0021] Preferably, the sintering temperature in step (2) is 1400-1650℃ and the sintering time is 4-10h.
[0022] Another aspect of the present invention provides a high-flowability oxide eutectic high-entropy ceramic powder, which is used as a raw material for laser additive manufacturing technology. Its excellent flowability ensures that the laser additive manufacturing process proceeds smoothly and normally.
[0023] The beneficial effects of this invention are:
[0024] 1. This invention provides high-quality raw materials for laser additive manufacturing technology by preparing high-entropy oxide eutectic ceramic powder with excellent flowability, ensuring the smoothness of the laser additive manufacturing process.
[0025] 2. The method of this invention successfully prepared high-flowability oxide eutectic high-entropy ceramic powder, providing high-quality raw materials for laser additive manufacturing technology. Attached Figure Description
[0026] Figure 1 This is a process flow diagram of the preparation method of the present invention.
[0027] Figure 2 This is a scanning electron microscope image of the oxide eutectic high-entropy ceramic powder prepared in Example 1 of the present invention.
[0028] Figure 3 The image shows the XRD pattern of the oxide eutectic high-entropy ceramic powder prepared in Example 1 of this invention.
[0029] Figure 4 This is a diagram showing the actual spraying effect of the oxide eutectic high-entropy ceramic powder prepared in Example 1 of the present invention. Detailed Implementation
[0030] The present invention will be further described in detail below with reference to specific embodiments.
[0031] Unless otherwise specified, all chemical reagents used in the embodiments and comparative examples of this invention were commercially available analytical grade reagents.
[0032] Example 1
[0033] (1) Commercially available Al2O3, Gd2O3, Nd2O3, Sm2O3, Eu2O3, and Er2O3 with particle sizes of 1–5 μm were used as initial raw material powders, wherein RE12O3 was Gd2O3, RE22O3 was Nd2O3, RE32O3 was Sm2O3, RE42O3 was Eu2O3, and RE52O3 was Er2O3. The molar ratio was...
[0034] The initial raw material powders, in a ratio of Al₂O₃:Gd₂O₃:Nd₂O₃:Sm₂O₃:Eu₂O₃:Er₂O₃ = 5:1:1:1:1:1, were weighed and ball-milled at 300 rpm for 12 hours using anhydrous ethanol as the medium to ensure thorough mixing. The mixed powders were then dried in an oven at 80°C for 4 hours. The dried powders were then ground in a mortar and passed through a 1000-mesh sieve. The sieved powders were then calcined in a muffle furnace at 1400°C for 8 hours. Finally, the calcined powders were passed through a 1000-mesh sieve to obtain a multi-principal-element solid-solution single-phase structure (Gd₂O₃:Nd₂O₃:Sm₂O₃:Eu₂O₃:Er₂O₃ = 5:1:1:1:1:1. 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Er 0.2 AlO3 high-entropy rare earth aluminate ceramic powder. Collect for later use.
[0035] (2) According to Al2O3:(Gd 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Er 0.2 Weigh alumina powder with a molar ratio of AlO3:ZrO2 = 39:38:23, and (5RE) 0.2 AlO3 powder and ZrO2 powder were mixed in anhydrous ethanol and ball-milled at 300 rpm for 12 hours using a planetary ball mill to ensure thorough mixing. The mixed powder was then dried in an oven at 80°C for 4 hours. The dried powder was then ground in a mortar and passed through a 1000-mesh sieve to obtain ternary eutectic high-entropy ceramic powder. This powder was poured into a stainless steel mold and pressed at 120 MPa for 3 minutes to obtain a blocky eutectic high-entropy ceramic preform. This preform was then placed in a muffle furnace and sintered at 1400°C for 10 hours to densify it, resulting in Al2O3 / (Gd) ceramic with a certain strength. 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Er 0.2 AlO3 / ZrO2 eutectic high-entropy ceramic sample.
[0036] (3) The Al2O3 / (Gd) obtained in step (2) 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Er 0.2 AlO3 / ZrO2 eutectic high-entropy ceramic samples were crushed in a mortar and sieved to collect powder particles of 15–75 μm, thus obtaining oxide eutectic high-entropy ceramic powder.
[0037] The Al2O3 / (Gd) prepared in this embodiment 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Er 0.2 Scanning electron microscopy (SEM) experiments were conducted on AlO3 / ZrO2 eutectic high-entropy ceramic powder, and the results are as follows: Figure 2 As shown; the phase analysis of the aforementioned ceramic powder was performed using XRD, and the results are as follows. Figure 3 As shown; the aforementioned ceramic powder is added as a raw material to the laser additive manufacturing equipment, and the actual situation of the raw material being delivered by the laser nozzle is as follows. Figure 4 As shown.
[0038] pass Figure 2 It can be seen that the oxide eutectic high-entropy ceramic powder prepared by this invention is in the form of irregularly shaped particles with good powder dispersion and no agglomeration. This proves that the oxide eutectic high-entropy ceramic powder prepared by this invention will not have its flowability affected by agglomeration, and its flowability can be maintained at an excellent level.
[0039] pass Figure 3 It can be seen that the oxide eutectic high-entropy ceramic powder prepared in this embodiment contains only Al2O3 and (Gd) 0.2 Nd 0.2 Sm 0.2 Eu 0.2 Er 0.2 The sample contained only AlO3 and ZrO2 phases, with no other impurities present. This indicates that the initial powders of the five rare earth oxides dissolved into the high-entropy rare earth aluminate phase as expected during the high-temperature solid-state reaction. Therefore, the method of this invention can successfully prepare oxide eutectic high-entropy ceramic powders.
[0040] pass Figure 4 As can be seen, the oxide eutectic high-entropy ceramic powder prepared in this embodiment can be uniformly and stably ejected from the laser nozzle without agglomeration, indicating that the oxide eutectic high-entropy ceramic powder prepared by this invention has excellent flowability and is suitable as a raw material for laser additive manufacturing technology.
[0041] Example 2
[0042] (1) Commercially available Al2O3, Y2O3, Er2O3, Yb2O3, Ho2O3, and Lu2O3 with particle sizes of 1–5 μm were used as initial raw material powders, wherein RE12O3 was Y2O3, RE22O3 was Er2O3, RE32O3 was Yb2O3, RE42O3 was Ho2O3, and RE52O3 was Lu2O3. The molar ratio was...
[0043] Al2O3:Y2O3:Er2O 3: Yb2O 3: Ho2O 3: The initial raw material powder (Lu₂O₃ = 5:1:1:1:1:1) was weighed and ball-milled at 300 rpm for 12 hours using anhydrous ethanol as the medium. The mixed powder was then placed in an oven and dried at 80°C for 6 hours. The dried powder was then ground in a mortar and passed through a 1000-mesh sieve. The sieved powder was then placed in a muffle furnace and calcined at 1600°C for 5 hours. The calcined powder was then passed through a 1000-mesh sieve to obtain a multi-principal-element solid solution single-phase structure (Y₂O₃). 0.2 Er 0.2 Yb 0.2 Ho 0.2 Lu 0.2 AlO3 high-entropy rare earth aluminate ceramic powder. Collect for later use.
[0044] (2) According to Al2O3:(Y 0.2 Er 0.2 Yb 0.2 Ho 0.2 Lu 0.2 Weigh alumina powder and (Y) in a molar ratio of AlO3 = 54:46. 0.2 Er 0.2 Yb 0.2 Ho 0.2 Lu 0.2 AlO3 powder was ball-milled at 300 rpm for 12 hours using anhydrous ethanol as the medium in a planetary ball mill to ensure thorough mixing. The thoroughly mixed powder was then dried in an oven at 80°C for 6 hours. The dried powder was then ground in a mortar and passed through a 1000-mesh sieve to obtain ternary eutectic high-entropy ceramic powder. This powder was poured into a stainless steel mold and pressed at 80 MPa for 5 minutes to obtain a blocky eutectic high-entropy ceramic preform. The preform was then placed in a muffle furnace and sintered at 1650°C for 4 hours to densify it, yielding Al2O3 / Y with a certain strength. 0.2 Er 0.2 Yb 0.2Ho 0.2 Lu 0.2 AlO3 eutectic high-entropy ceramic sample.
[0045] (3) The Al2O3 / Y obtained in step (2) 0.2 Er 0.2 Yb 0.2 Ho 0.2 Lu 0.2 AlO3 eutectic high-entropy ceramic samples were crushed in a mortar and sieved to collect powder particles of 15–75 μm, thus obtaining oxide eutectic high-entropy ceramic powder.
[0046] The oxide eutectic high-entropy ceramic powder prepared in this embodiment has similar properties to that in Example 1.
[0047] Example 3
[0048] (1) Commercially available Al₂O₃, Gd₂O₃, Y₂O₃, Ho₂O₃, Yb₂O₃, and Er₂O₃ powders with particle sizes of 1–5 μm were used as initial raw material powders, wherein RE₁₂O₃ was Gd₂O₃, RE₂₂O₃ was Y₂O₃, RE₃₂O₃ was Ho₂O₃, RE₄₂O₃ was Yb₂O₃, and RE₅₂O₃ was Er₂O₃. The molar ratio was...
[0049] The initial raw material powders, in a ratio of Al₂O₃:Gd₂O₃:Y₂O₃:Ho₂O₃:Yb₂O₃:Er₂O₃ = 25:3:3:3:3, were weighed. Using anhydrous ethanol as the medium, the weighed mixed powders were ball-milled at 300 rpm for 12 hours to ensure thorough mixing. Then, the mixed powders were placed in an oven and dried at 80°C for 5 hours. The dried mixed powders were then ground in a mortar and passed through a 1000-mesh sieve. The sieved mixed powders were then placed in a muffle furnace and calcined at 1500°C for 6 hours. Finally, the calcined mixed powders were passed through a 1000-mesh sieve to obtain a multi-principal-element solid solution single-phase structure (Gd₂O₃:Ho₂O₃:Yb₂O₃:Er₂O₃ = 25:3:3:3:3. 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 High-entropy rare-earth aluminate ceramic powder. Collect for later use.
[0050] (2) According to Al2O3:(Gd 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 Weigh alumina powder with a molar ratio of ZrO2 = 38.3:10.7:19.0, and (Gd 0.2 Y0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 Powdered ZrO2 and ZrO2 were ball-milled at 300 rpm for 12 hours using anhydrous ethanol as the medium in a planetary ball mill to ensure thorough mixing. The thoroughly mixed powder was then dried in an oven at 80°C for 5 hours. The dried powder was then ground in a mortar and passed through a 1000-mesh sieve to obtain ternary eutectic high-entropy ceramic powder. The ternary eutectic high-entropy ceramic powder was poured into a stainless steel mold and pressed at 100 MPa for 4 minutes to obtain a blocky eutectic high-entropy ceramic preform. The blocky eutectic high-entropy ceramic preform was then placed in a muffle furnace and sintered at 1500°C for 8 hours to densify it, yielding Al2O3 / (Gd) ceramic with a certain strength. 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 / ZrO2 eutectic high-entropy ceramic sample.
[0051] (3) The Al2O3 / (Gd) obtained in step (2) 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 The ZrO2 eutectic high-entropy ceramic sample was crushed in a mortar and sieved to collect powder particles of 15–75 μm, thus obtaining oxide eutectic high-entropy ceramic powder.
[0052] The oxide eutectic high-entropy ceramic powder prepared in this embodiment has similar properties to that in Example 1.
[0053] Example 4
[0054] (1) Commercially available Al₂O₃, Gd₂O₃, Y₂O₃, Ho₂O₃, Yb₂O₃, and Er₂O₃ powders with particle sizes of 1–5 μm were used as initial raw material powders, wherein RE₁₂O₃ was Gd₂O₃, RE₂₂O₃ was Y₂O₃, RE₃₂O₃ was Ho₂O₃, RE₄₂O₃ was Yb₂O₃, and RE₅₂O₃ was Er₂O₃. The molar ratio was...
[0055] The initial raw material powders, in a ratio of Al₂O₃:Gd₂O₃:Y₂O₃:Ho₂O₃:Yb₂O₃:Er₂O₃ = 25:3:3:3:3:3, were weighed. Using anhydrous ethanol as the medium, the weighed mixed powders were ball-milled at 300 rpm for 12 hours to ensure thorough mixing. Then, the mixed powders were placed in an oven and dried at 80°C for 5 hours. The dried mixed powders were then ground in a mortar and passed through a 1000-mesh sieve. The sieved mixed powders were then placed in a muffle furnace and calcined at 1450°C for 7 hours. Finally, the calcined mixed powders were passed through a 1000-mesh sieve to obtain a multi-principal-element solid solution single-phase structure (Gd₂O₃:Yb₂O₃:Ho₂O₃:Yb₂O₃:Er₂O₃ = 25:3:3:3:3:3. 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 High-entropy rare-earth aluminate ceramic powder. Collect for later use.
[0056] (2) According to Al2O3:(Gd 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 Weigh alumina powder and (Gd) in a molar ratio of 52:12. 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 The powder, using anhydrous ethanol as the medium, was ball-milled at 300 rpm for 12 hours using a planetary ball mill to ensure thorough mixing. The thoroughly mixed powder was then dried in an oven at 80°C for 5 hours. The dried powder was then ground in a mortar and passed through a 1000-mesh sieve to obtain binary eutectic high-entropy ceramic powder. This powder was poured into a stainless steel mold and pressed at 120 MPa for 4 minutes to obtain a blocky eutectic high-entropy ceramic preform. This preform was then placed in a muffle furnace and sintered at 1600°C for 6 hours to densify it, yielding Al₂O₃ / (Gd ... 0.2 Y 0.2 Ho 0.2 Yb 0.2 Er 0.2 )3Al5O 12 Eutectic high-entropy ceramic sample.
[0057] (3) The Al2O3 / (Gd) obtained in step (2) 0.2 Y 0.2 Ho0.2 Yb 0.2 Er 0.2 )3Al5O 12 The eutectic high-entropy ceramic sample was crushed in a mortar and sieved to collect powder particles of 15–75 μm, thus obtaining oxide eutectic high-entropy ceramic powder.
[0058] The oxide eutectic high-entropy ceramic powder prepared in this embodiment has similar properties to that in Example 1.
[0059] In summary, the method of this invention can successfully prepare oxide eutectic high-entropy ceramic powder. Furthermore, the oxide eutectic high-entropy ceramic powder prepared by this invention can be used as a raw material for laser additive manufacturing technology. Utilizing its high fluidity, the laser nozzle can uniformly and stably eject the oxide eutectic high-entropy ceramic powder, thereby ensuring the smoothness and stability of the laser additive manufacturing process.
[0060] Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made to it in form and detail without departing from the scope defined by the claims of the present invention.
Claims
1. A method for preparing a high-flowability oxide eutectic high-entropy ceramic powder, characterized in that: The preparation method includes the following steps: (1) Preparation of multi-principal element solid solution single-phase high-entropy rare earth aluminate ceramic powder: The initial raw material powder is weighed with a molar ratio of Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3=25:3:3:3:3:3 or Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3=5:1:1:1:1:
1. The initial raw material powder is mixed by wet ball milling, dried, and then ground and passed through a 1000-mesh sieve. The mixed powder obtained after sieving is calcined and then passed through a 1000-mesh sieve to obtain multi-principal element solid solution single-phase high-entropy rare earth aluminate ceramic powder for later use. The chemical formula of multi-principal element solid solution single-phase high-entropy rare earth aluminate ceramic powder is denoted as (5RE) depending on the molar ratio of the initial raw material powder. 0.2 )3Al5O 12 or (5RE) 0.2 AlO3; (2) Preparation of oxide eutectic high-entropy ceramic samples: according to the molar ratio of Al2O3:(5RE) 0.2 )3Al5O 12 =52:12 or Al2O3:(5RE) 0.2 Weigh alumina powder (AlO3=54:46) and the multi-principal solid solution single-phase high-entropy rare earth aluminate ceramic powder prepared in step (1). Weigh the Al2O3 powder and (5RE) powder. 0.2 )3Al5O 12 or (5RE) 0.2 After the AlO3 powder is thoroughly mixed, it is dried, ground, and sieved to obtain binary eutectic high-entropy ceramic powder. According to the molar ratio Al2O3:(5RE) 0.2 )3Al5O 12 ZrO2 = 38.3:10.7:19.0 or Al2O3:(5RE) 0.2 AlO3:ZrO2 = 39:38:
23. Weigh alumina powder, multi-principal component solid solution single-phase high-entropy rare earth aluminate ceramic powder, and ZrO2 powder. After thoroughly mixing the weighed alumina powder, multi-principal component solid solution single-phase high-entropy rare earth aluminate ceramic powder, and ZrO2 powder, dry, grind, and sieve to obtain ternary eutectic high-entropy ceramic powder. Binary eutectic high-entropy ceramic powder or ternary eutectic high-entropy ceramic powder is poured into a stainless steel mold and pressed to obtain a blocky eutectic high-entropy ceramic preform. The blocky eutectic high-entropy ceramic preform is then sintered at high temperature to obtain an alumina-based eutectic high-entropy ceramic sample. (3) Preparation of oxide eutectic high-entropy ceramic powder: After crushing and sieving the alumina-based eutectic high-entropy ceramic sample obtained in step (2), collect powder particles with a particle size of 15~75μm to obtain oxide eutectic high-entropy ceramic powder. For powder particles with a particle size greater than the upper limit, continue to crush and sieve until the particle size meets the requirements. For powder particles with a particle size less than the lower limit, re-press, sinter, crush and sieve until the particle size meets the requirements.
2. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: RE12O3 to RE52O3 are five rare earth oxides with the same crystal structure and ionic radii differing by less than 10%. RE represents rare earth elements, including Sc, Y, and lanthanides.
3. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 2, characterized in that: In step (1), the particle size of Al2O3 powder and rare earth oxide powder are both 1~5μm.
4. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: In step (1), the wet ball milling medium is anhydrous ethanol, the wet ball milling speed is 300 r / min, and the ball milling time is 12 h.
5. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: In step (1), the drying temperature is 80℃ and the heat preservation time is 4~6h.
6. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: In step (1), the calcination temperature is 1400~1600℃ and the calcination time is 5~8h.
7. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: In step (1), when the molar ratio is Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3=25:3:3:3:3:3, the prepared high-entropy rare-earth aluminate ceramic powder has a garnet structure; when the molar ratio is Al2O3:RE12O3:RE22O3:RE32O3:RE42O3:RE52O3=5:1:1:1:1:1, the prepared high-entropy rare-earth aluminate ceramic powder has a perovskite structure. In step (2), when the high-entropy rare-earth aluminate ceramic powder has a garnet structure, the molar ratio Al2O3:(5RE) is... 0.2 )3Al5O 12 =52:12, molar ratio Al2O3:(5RE) 0.2 )3Al5O 12 ZrO2 = 38.3:10.7:19.0; When the high-entropy rare-earth aluminate ceramic powder has a perovskite structure, the molar ratio Al2O3:(5RE) is 38.3:10.7:19.
0. 0.2 AlO3 = 54:46, molar ratio Al2O3:(5RE) 0.2 AlO3:ZrO2 = 39:38:
23.
8. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: In step (2), the pressure for pressing the blocky eutectic high-entropy ceramic preform is 80~120MPa, and the holding time is 3~5min.
9. The method for preparing a high-flowability oxide eutectic high-entropy ceramic powder according to claim 1, characterized in that: In step (2), the sintering temperature is 1400~1650℃ and the sintering time is 4~10h.
10. A high-flowability oxide eutectic high-entropy ceramic powder, characterized in that: It is prepared according to the preparation method according to any one of claims 1-9.
Citation Information
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