Nanoparticulate agglomerated rare earth doped YSZ powder and method of making same

Abstract

The present disclosure provides a kind of nanometer agglomerated rare earth doped YSZ powder and its preparation method, it is related to ceramic powder preparation technical field.The preparation method includes: using dispersant to carry out surface modification treatment to metal ion solution, to obtain reaction solution;Wherein, metal ion solution includes zirconium salt, yttrium salt and at least one rare earth salt except yttrium salt;Reaction solution is carried out aging treatment, ultrasonic treatment and drying treatment, to obtain rare earth doped YSZ precursor powder;Rare earth doped YSZ precursor powder is carried out at least two calcination treatments, to obtain rare earth doped YSZ nano powder;Rare earth doped YSZ nano powder is matched with deionized water into slurry, and slurry is carried out ball milling, to obtain rare earth doped YSZ agglomerate;Rare earth doped YSZ agglomerate is carried out at least two sintering treatments, to obtain intermediate powder;Intermediate powder is sieved, to obtain nanometer agglomerated rare earth doped YSZ powder.The present disclosure can improve YSZ material performance.

Description

Technical Field

[0001] This disclosure relates to the field of ceramic powder preparation technology, and more specifically, to a method for preparing nano-agglomerated rare earth-doped YSZ powder and the nano-agglomerated rare earth-doped YSZ powder. Background Technology

[0002] Thermal barrier coatings are widely used in high-temperature components such as aero-engines, combustion chambers, and spacecraft to effectively reduce high-temperature damage to materials and extend the service life of workpieces. Yttria-stabilized zirconia (YSZ) is widely used in thermal barrier coatings due to its excellent properties such as low thermal conductivity, high coefficient of thermal expansion, and good chemical stability.

[0003] However, when the operating temperature is above 1200℃ for a long time, the YSZ material will undergo a transformation from a tetragonal phase to a monoclinic phase, causing the thermal barrier coating to expand in volume, resulting in cracks in the coating and ultimately causing it to peel off and fail.

[0004] To address the aforementioned issues, some technologies have improved the lifetime of YSZ coatings through rare-earth doping. Currently, the preparation process of rare-earth-doped YSZ powder mainly relies on ball milling of oxide powders to achieve rare-earth doping through solid-state diffusion. However, this method makes it difficult to ensure that rare-earth elements completely enter the zirconium oxide lattice, resulting in insufficient performance of rare-earth-doped YSZ materials.

[0005] It should be noted that the information disclosed in the background section above is only used to enhance the understanding of the background of this disclosure, and therefore may include information that does not constitute prior art known to those skilled in the art. Summary of the Invention

[0006] The purpose of this disclosure is to provide a method for preparing nano-agglomerated rare earth-doped YSZ powder and the nano-agglomerated rare earth-doped YSZ powder, thereby overcoming, at least to some extent, the problem of insufficient performance of YSZ materials.

[0007] According to a first aspect of this disclosure, a method for preparing nano-agglomerated rare earth-doped YSZ powder is provided, comprising: surface modification treatment of a metal ion solution using a dispersant to obtain a reaction solution; wherein the metal ion solution comprises zirconium salt, yttrium salt, and at least one rare earth salt other than yttrium salt; aging, ultrasonicating, and drying the reaction solution to obtain rare earth-doped YSZ precursor powder; calcining the rare earth-doped YSZ precursor powder at least twice to obtain rare earth-doped YSZ nanopowder; preparing a slurry from the rare earth-doped YSZ nanopowder with deionized water, and ball milling the slurry to obtain rare earth-doped YSZ agglomerates; sintering the rare earth-doped YSZ agglomerates at least twice to obtain an intermediate powder; and sieving the intermediate powder to obtain nano-agglomerated rare earth-doped YSZ powder.

[0008] Optionally, the surface modification treatment of the metal ion solution using a dispersant to obtain a reaction solution includes: adding the metal ion solution and the dispersant to an impinging flow reactor containing deionized water; adding a precipitant dropwise to the impinging flow reactor, and combining the stirring and ultrasonic operation of the impinging flow reactor to obtain the reaction solution; wherein the precipitant is used to adjust the pH of the solution.

[0009] Optionally, the precipitant is one or more of ammonium bicarbonate, ammonium hydroxide, and urea; wherein the pH of the reaction solution is adjusted to 8 to 11.

[0010] Optionally, the stirring speed of the impinging flow reactor is from 400 r / min to 2000 r / min, and the ultrasonic power is from 10 kHz to 100 kHz.

[0011] Optionally, the zirconium salt is zirconium nitrate or zirconium dichloride, the yttrium salt is yttrium nitrate or yttrium chloride, and the rare earth salt includes gadolinium salt and / or ytterbium salt, wherein the gadolinium salt is gadolinium nitrate or gadolinium chloride, and the ytterbium salt is ytterbium nitrate or ytterbium chloride; the dispersant is one or a mixture of polyvinylpyrrolidone, hexadecyltrimethylammonium bromide, polyethylene glycol ethoxylates, and polyethylene glycol.

[0012] Optionally, the reaction solution is subjected to aging, ultrasonic treatment, and drying to obtain rare earth-doped YSZ precursor powder, including: aging the reaction solution to obtain a first solution; ultrasonically dispersing the first solution using an ultrasonic cell disruptor to obtain a second solution; the frequency of the ultrasonic cell disruptor is 10 kHz to 100 kHz, and the ultrasonic time is 10 min to 200 min; drying the second solution using a vacuum freeze dryer to obtain rare earth-doped YSZ precursor powder; the drying time of the vacuum freeze dryer is 10 h to 24 h.

[0013] Optionally, the calcination temperature of each of the at least two calcination treatments is 400°C to 800°C, and the calcination time of each calcination treatment is 1 hour to 10 hours.

[0014] Optionally, the sintering temperature of each of the at least two sintering processes is between 900°C and 1300°C, and the sintering time of each process is between 2 hours and 10 hours.

[0015] Optionally, sieving the intermediate powder includes sieving the intermediate powder based on a sieving operation with a sieve size of 200 to 1000 mesh.

[0016] According to a second aspect of this disclosure, a nano-agglomerated rare earth-doped YSZ powder is provided, which is prepared by any of the above-described methods for preparing nano-agglomerated rare earth-doped YSZ powder.

[0017] The preparation method of nano-agglomerated rare earth-doped YSZ powder according to the present disclosure has several advantages. First, by incorporating rare earth elements into YSZ through a metal salt solution deposition reaction, the rare earth elements can be incorporated into the zirconium oxide lattice, effectively improving the high-temperature performance of the material and thus helping to extend the lifespan of the coating prepared from it. Second, the metal salt solution reaction combined with a dispersant and at least two calcination treatments of the present disclosure help to obtain highly dispersed and uniform nano-powder. Third, the at least two sintering treatments of the present disclosure can achieve densification of rare earth-doped YSZ nano-powder while maintaining uniformity. Fourth, the preparation method of the present disclosure has high processing efficiency, simple operation, low cost, and is easy to industrialize.

[0018] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit this disclosure. Attached Figure Description

[0019] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this disclosure and, together with the description, serve to explain the principles of this disclosure. It is obvious that the drawings described below are merely some embodiments of this disclosure, and those skilled in the art can obtain other drawings based on these drawings without any inventive effort.

[0020] Figure 1 A flowchart illustrating a method for preparing nano-agglomerated rare earth-doped YSZ powder according to an exemplary embodiment of the present disclosure is shown.

[0021] Figure 2 The XRD (X-Ray Diffractometer) pattern of the rare earth-doped YSZ nanopowder of Embodiment 1 of this disclosure is shown.

[0022] Figure 3 A scanning electron microscope image of rare earth-doped YSZ nanopowder of Embodiment 1 of this disclosure is shown.

[0023] Figure 4 The XRD pattern of the nano-agglomerated rare earth-doped YSZ powder of Embodiment 1 of this disclosure is shown.

[0024] Figure 5 A scanning electron microscope image of the nano-agglomerated rare earth-doped YSZ powder of Embodiment 1 of this disclosure is shown. Detailed Implementation

[0025] Exemplary embodiments will now be described more fully with reference to the accompanying drawings. However, these exemplary embodiments can be implemented in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided to make this disclosure more comprehensive and complete, and to fully convey the concept of the exemplary embodiments to those skilled in the art. The described features, structures, or characteristics can be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a full understanding of embodiments of this disclosure. However, those skilled in the art will recognize that the technical solutions of this disclosure can be practiced with one or more of these specific details omitted, or other methods, processes, steps, etc., can be employed. In other instances, well-known technical solutions are not shown or described in detail to avoid obscuring various aspects of this disclosure.

[0026] Furthermore, the accompanying drawings are merely illustrative of this disclosure and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and therefore repeated descriptions of them will be omitted. The flowcharts shown in the drawings are merely exemplary illustrations and do not necessarily include all steps. For example, some steps may be broken down, while others may be combined or partially combined; therefore, the actual order of execution may change depending on the actual situation. Additionally, all terms such as "first," "second," etc., used below are for distinction purposes only and should not be construed as limiting the content of this disclosure.

[0027] Figure 1 A flowchart illustrating a method for preparing nano-agglomerated rare-earth-doped YSZ powder according to an exemplary embodiment of this disclosure is shown. Reference Figure 1 The preparation method of nano-agglomerated rare earth-doped YSZ powder according to the present disclosure includes the following steps:

[0028] S102. A surface modification treatment is performed on a metal ion solution using a dispersant to obtain a reaction solution; wherein the metal ion solution contains zirconium salt, yttrium salt, and at least one rare earth salt other than yttrium salt.

[0029] In exemplary embodiments of this disclosure, the metal ion solution may comprise zirconium salt, yttrium salt, and at least one rare earth salt other than yttrium salt. Specifically, the zirconium salt may be zirconium nitrate (Zr(NO3)4·H2O) or zirconium oxychloride (ZrOCl2·8H2O); the yttrium salt may be yttrium nitrate (Y(NO3)3·H2O) or yttrium chloride (YCl3·6H2O); and the rare earth salt may include gadolinium salt and / or ytterbium salt, wherein the gadolinium salt may be gadolinium nitrate (Gd(NO3)3·H2O) or gadolinium chloride (GdCl3·6H2O), and the ytterbium salt may be ytterbium nitrate (Yb(NO3)3·H2O) or ytterbium chloride (YbCl3·6H2O).

[0030] In addition, the dispersant used in this disclosure may be one or a mixture of polyvinylpyrrolidone, hexadecyltrimethylammonium bromide, polyethylene glycol ethoxylates, and polyethylene glycol.

[0031] It should be understood that the zirconium salt, yttrium salt, and at least one rare earth salt other than yttrium salt contained in the above-mentioned dispersant and metal ion solution are merely illustrative examples and are not intended to limit the scope of this disclosure.

[0032] According to some embodiments of this disclosure, a dispersant and a metal ion solution can be added to a container and mixed by heating and ultrasonic treatment to obtain a reaction solution.

[0033] According to other embodiments of this disclosure, the pH of the solution can be adjusted by regulating the rotational speed and ultrasonic power of the impinging flow reactor and the type of precipitant to obtain the reaction solution.

[0034] Specifically, a metal ion solution and a dispersant can be added to an impinging flow reactor containing deionized water, and a precipitant can be added dropwise to the impinging flow reactor. The reaction solution is obtained by combining the stirring and ultrasonic operation of the impinging flow reactor.

[0035] The precipitant can be used to adjust the pH of the solution, and can specifically be one or a mixture of ammonium bicarbonate, ammonium hydroxide, and urea. Furthermore, the pH of the resulting reaction solution is adjusted to between 8 and 11.

[0036] To achieve good dispersibility, high purity, and size uniformity, these embodiments employed a combination of dispersant modification, adjustment of the impinging flow reactor rotation speed, and ultrasonic power. Specifically, the impinging flow reactor rotation speed ranged from 400 r / min to 2000 r / min, and the ultrasonic power ranged from 10 kHz to 100 kHz.

[0037] S104. The reaction solution is subjected to aging, ultrasonic treatment and drying to obtain rare earth-doped YSZ precursor powder.

[0038] After obtaining the reaction solution in step S102, the reaction solution can be aged. This disclosure does not limit the aging time, for example, it can be 10 hours to 30 hours. In this embodiment, the solution obtained after aging is referred to as the first solution.

[0039] Next, the first solution can be ultrasonically dispersed using an ultrasonic cell disruptor to obtain the second solution. The frequency of the ultrasonic cell disruptor is 10 kHz to 100 kHz, and the ultrasonic treatment time is 10 min to 200 min.

[0040] Subsequently, the second solution can be dried using a vacuum freeze dryer to obtain rare earth-doped YSZ precursor powder. The drying time in the vacuum freeze dryer is 10 to 24 hours.

[0041] S106. The rare earth-doped YSZ precursor powder is subjected to at least two calcination treatments to obtain rare earth-doped YSZ nanopowder.

[0042] After obtaining the rare earth-doped YSZ precursor powder in step S104, the powder can be subjected to multiple calcination treatments. This disclosure does not limit the number of calcination treatments. The calcination temperature for each treatment is between 400°C and 800°C, and the calcination time for each treatment is between 1 hour and 10 hours.

[0043] It should be noted that in some embodiments of this disclosure, the temperature of each calcination treatment may be higher than the temperature of the previous calcination treatment; for example, the temperature of the second calcination treatment may be higher than the temperature of the first calcination treatment. However, in other embodiments of this disclosure, each calcination treatment is considered an independent process, and its temperature is not limited by the temperatures of other calcination treatments.

[0044] S108. Rare earth-doped YSZ nanopowder is mixed with deionized water to form a slurry, and the slurry is ball-milled to obtain rare earth-doped YSZ agglomerates.

[0045] In an exemplary embodiment of this disclosure, the slurry concentration is configured to be from 10 wt% to 50 wt%. The ball milling time can be configured to be from 0.5 h to 5 h. Furthermore, this disclosure does not limit the ball milling process; for example, alumina balls and an alumina ball milling jar may be used for ball milling. This disclosure does not limit the diameter of the alumina balls, the ball-to-material ratio, the rotational speed of the ball milling process, or the ball milling time.

[0046] S110. The rare earth-doped YSZ agglomerates are subjected to at least two sintering processes to obtain intermediate powder.

[0047] After obtaining the rare earth-doped YSZ agglomerates in step S108, the agglomerates can be subjected to multiple sintering processes. This disclosure does not limit the number of sintering processes. The sintering temperature for each sintering process is between 900°C and 1300°C, and the sintering time for each sintering process is between 2 hours and 10 hours.

[0048] Taking a two-stage sintering process as an example, the first sintering process yields a porous sample with a high grain growth index and good microstructure uniformity. The second sintering process allows the sintered body to achieve densification through grain boundary diffusion, preventing further grain growth. Therefore, by controlling the sintering temperature and time, material densification can be achieved while maintaining uniformity.

[0049] S112. The intermediate powder is sieved to obtain nano-agglomerated rare earth-doped YSZ powder.

[0050] In an exemplary embodiment of this disclosure, the intermediate powder obtained after sintering is sieved to obtain the nano-agglomerated rare earth-doped YSZ powder described in this disclosure. Specifically, the intermediate powder can be sieved using a sieve with a mesh size of 200 to 1000 mesh.

[0051] The powder obtained from the preparation process of steps S102 to S112 has a flowability of 50s / 50g to 54s / 50g and a bulk density of 1.8g / cc to 2.0g / cc.

[0052] The preparation process of the nano-agglomerated rare earth-doped YSZ powder disclosed herein will be described in detail below through examples.

[0053] Example 1

[0054] A method for preparing nano-agglomerated rare earth-doped YSZ powder with a material composition of 5.0 mol% Gd₂O₃: 6.0 mol% Yb₂O₃: 9 mol% Y₂O₃: 80.0 mol% ZrO₂, abbreviated as 5Gd₆Yb₉YSZ, is provided, comprising the following steps:

[0055] Step 1: Calculate the masses of Gd(NO3)3·H2O, Yb(NO3)3·H2O, Y(NO3)3·H2O, and Zr(NO3)4·H2O based on the molar ratio of Gd2O3:Yb2O3:Y2O3:ZrO2 (5:6:9:80). This yields a metal ion solution with these compositions. This solution is then added to an impinging flow reactor containing 200 mL of deionized water to achieve a concentration of 0.15 mol / L. 0.5 wt% polyvinylpyrrolidone dispersant is added, and the mixture is stirred until clear. The impinging flow reactor is stirred at 800 r / min, with an ultrasonic power of 20 kHz. 0.5 mol / L ammonium hydroxide solution is added dropwise at a rate of 5 mL / min to bring the pH of the solution to 11. This yields the reaction solution described in this disclosure.

[0056] Step 2: The reaction solution obtained in Step 1 was aged for 10 hours, then ultrasonically dispersed at a frequency of 20 kHz for 20 minutes using an ultrasonic cell disruptor, and dried using a vacuum freeze dryer for 10 hours to obtain 5Gd6Yb9YSZ precursor powder.

[0057] Step 3: Calcine the precursor powder obtained in Step 2 at 400℃ for 1 hour, and then at 800℃ for 1 hour to obtain 5Gd6Yb9YSZ nanopowder with high dispersibility, high purity and size uniformity.

[0058] Figure 2 The XRD spectrum of the 5Gd6Yb9YSZ nanopowder is shown, with reference to... Figure 2 It can be seen that the nanopowder has no diffraction peaks for Gd2O3, Yb2O3, and Y2O3, indicating that Gd2O3 is not present in the nanopowder. 3+ Yb 3+ and Y 3+ Uniformly dispersed in the gel, and respectively replacing Zr 4+ It forms a substitutional solid solution and exists stably in the form of a single tetragonal phase.

[0059] Figure 3 The corresponding scanning micrograph is shown for reference. Figure 2 It can be seen that the 5Gd6Yb9YSZ nanopowder obtained in this step has high dispersibility and size uniformity.

[0060] Step 4: Prepare a 10wt% slurry from the 5Gd6Yb9YSZ nanopowder obtained in Step 3, ball mill it for 0.5 h, and then spray dry it.

[0061] Step 5: The sample spray-dried in Step 4 is sintered at 1200℃ for 1 hour, followed by sintering at 1100℃ for 10 hours to obtain densified 5Gd6Yb9YSZ nano-agglomerated rare earth doped YSZ powder.

[0062] Figure 4 The XRD spectrum of the 5Gd6Yb9YSZ nano-agglomerated powder is shown, with reference to... Figure 2 It can be seen that the nanopowder still exists stably as a single tetragonal phase of ZrO2, while its crystallinity is significantly improved.

[0063] Step 6: The densified powder obtained in Step 5 is sieved through 325 mesh and 800 mesh to obtain 5Gd6Yb9YSZ nano-agglomerated rare earth doped YSZ powder with a size of 18μm to 45μm.

[0064] Figure 5 Scanning micrographs of the nano-agglomerated rare-earth-doped YSZ powder of Embodiment 1 of this disclosure are shown, wherein images a and b are observed at different scales: image a is at a scale of 200 μm, and image b is at a scale of 100 μm. See also Figure 5 As can be seen, the powder has good sphericity. Furthermore, its flowability is 50s / 50g, and its loose packing density is 2.0g / cc.

[0065] Example 2

[0066] A method for preparing nano-agglomerated rare earth-doped YSZ powder with a material composition of 4.0 mol% Gd₂O₃: 5.0 mol% Yb₂O₃: 8 mol% Y₂O₃: 83.0 mol% ZrO₂, abbreviated as 4Gd₅Yb₈YSZ, is provided, comprising the following steps:

[0067] Step 1: Calculate the masses of GdCl3·6H2O, YbCl3·6H2O, YCl3·6H2O, and ZrOCl2·8H2O based on the molar ratio of Gd2O3:Yb2O3:Y2O3:ZrO2 (4:5:8:83). This yields a metal ion solution with these compositions. Add this metal ion solution to an impinging flow reactor containing 200 mL of deionized water to achieve a concentration of 0.3 mol / L. Add 1 wt% hexadecyltrimethylammonium bromide dispersant and stir until clear. The impinging flow reactor is stirred at 1000 r / min, with an ultrasonic power of 30 kHz. Add 0.5 mol / L ammonium bicarbonate solution dropwise at a rate of 10 mL / min to adjust the pH to 10. This yields the reaction solution described in this disclosure.

[0068] Step 2: The reaction solution obtained in Step 1 was aged for 15 hours, then ultrasonically dispersed at a frequency of 30 kHz for 30 minutes using an ultrasonic cell disruptor, and dried using a vacuum freeze dryer for 15 hours to obtain 4Gd5Yb8YSZ precursor powder.

[0069] Step 3: Calcine the precursor powder obtained in Step 2 at 500℃ for 2 hours, and then at 700℃ for 2 hours to obtain 4Gd5Yb8YSZ nanopowder with high dispersibility, high purity and size uniformity.

[0070] Step 4: Prepare a 40wt% slurry from the 4Gd5Yb8YSZ nanopowder obtained in Step 3, ball mill it for 1 hour, and then spray dry it.

[0071] Step 5: The sample spray-dried in Step 4 is sintered at 1100℃ for 2 hours, followed by sintering at 1000℃ for 5 hours to obtain densified 4Gd5Yb8YSZ nano-agglomerated rare earth doped YSZ powder.

[0072] Step 6: The densified powder obtained in Step 5 is sieved through 200 mesh and 600 mesh to obtain 4Gd5Yb8YSZ nano-agglomerated rare earth-doped YSZ powder with a size of 23μm to 75μm. Its flowability is measured to be 54s / 50g, and its bulk density is 1.8g / cc.

[0073] Example 3

[0074] A method for preparing nano-agglomerated rare earth-doped YSZ powder with a material composition of 3.0 mol% Gd₂O₃: 3.0 mol% Yb₂O₃: 4 mol% Y₂O₃: 90.0 mol% ZrO₂, abbreviated as 3Gd₃Yb₄YSZ, is provided, comprising the following steps:

[0075] Step 1: Calculate the masses of Gd(NO3)3·H2O, Yb(NO3)3·H2O, Y(NO3)3·H2O, and Zr(NO3)4·H2O based on the molar ratio of Gd2O3:Yb2O3:Y2O3:ZrO2 (3:3:4:90). This yields a metal ion solution with these compositions. This solution is then added to an impinging flow reactor containing 200 mL of deionized water to achieve a concentration of 0.5 mol / L. 0.5 wt% polyethylene glycol ethoxylate dispersant is added and the mixture is stirred until clear. The impinging flow reactor is stirred at 2000 r / min, with an ultrasonic power of 20 kHz. A 0.5 mol / L urea solution is added dropwise at a rate of 5 mL / min to adjust the pH to 8. This yields the reaction solution described in this disclosure.

[0076] Step 2: The reaction solution obtained in Step 1 was aged for 24 hours, then ultrasonically dispersed at a frequency of 70 kHz for 40 minutes using an ultrasonic cell disruptor, and dried using a vacuum freeze dryer for 24 hours to obtain 3Gd3Yb4YSZ precursor powder.

[0077] Step 3: The precursor powder obtained in Step 2 was calcined at 400℃ for 1 h, followed by calcination at 700℃ for 6 h to obtain 3Gd3Yb4YSZ nanopowder with high dispersibility, high purity and size uniformity.

[0078] Step 4: Prepare a slurry with a concentration of 25wt% using the 3Gd3Yb4YSZ nanopowder obtained in Step 3, ball mill it for 0.5h, and then spray dry it.

[0079] Step 5: The sample spray-dried in Step 4 is sintered at 1300℃ for 1 hour, followed by sintering at 900℃ for 10 hours to obtain densified 3Gd3Yb4YSZ nano-agglomerated rare earth doped YSZ powder.

[0080] Step 6: The densified powder obtained in Step 5 is sieved through 300 mesh and 1000 mesh to obtain 3Gd3Yb4YSZ nano-agglomerated rare earth-doped YSZ powder with a size of 13μm to 48μm. Its flowability is measured to be 52s / 50g, and its bulk density is 1.94g / cc.

[0081] Furthermore, this disclosure also provides a nano-agglomerated rare earth-doped YSZ powder, which is prepared using the above-described method for preparing nano-agglomerated rare earth-doped YSZ powder.

[0082] Furthermore, this disclosure also provides a thermal barrier coating prepared using the aforementioned nano-agglomerated rare earth-doped YSZ powder.

[0083] It should be noted that although the steps of the method in this disclosure are described in a specific order in the accompanying drawings, this does not require or imply that the steps must be performed in that specific order, or that all the steps shown must be performed to achieve the desired result. Additional or alternative steps may be omitted, multiple steps may be combined into one step, and / or a step may be broken down into multiple steps.

[0084] Furthermore, the above figures are merely illustrative of the processes included in the method according to exemplary embodiments of this disclosure and are not intended to be limiting. It is readily understood that the processes shown in the above figures do not indicate or limit the temporal order of these processes. Additionally, it is readily understood that these processes may be executed synchronously or asynchronously, for example, in multiple modules.

[0085] Other embodiments of this disclosure will readily occur to those skilled in the art upon consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of this disclosure that follow the general principles of this disclosure and include common knowledge or customary techniques in the art not disclosed herein. The specification and examples are to be considered exemplary only, and the true scope and spirit of this disclosure are indicated by the claims.

[0086] It should be understood that this disclosure is not limited to the precise structures described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of this disclosure is limited only by the appended claims.

Claims

1. A method for preparing nano-agglomerated rare earth-doped YSZ powder, characterized in that, include: A surface modification treatment of a metal ion solution is performed using a dispersant to obtain a reaction solution; wherein the metal ion solution contains zirconium salt, yttrium salt, and at least one rare earth salt other than the yttrium salt. The reaction solution is aged to obtain a first solution; the first solution is ultrasonically dispersed using an ultrasonic cell disruptor to obtain a second solution; the frequency of the ultrasonic cell disruptor is 10 kHz to 100 kHz, and the ultrasonic time is 10 min to 200 min; the second solution is dried using a vacuum freeze dryer to obtain rare earth-doped YSZ precursor powder; the drying time of the vacuum freeze dryer is 10 h to 24 h. The rare earth-doped YSZ precursor powder is subjected to at least two calcination treatments to obtain rare earth-doped YSZ nanopowder; the calcination temperature of each of the at least two calcination treatments is 400℃ to 800℃, and the calcination time of each calcination treatment is 1h to 10h. The rare earth-doped YSZ nanopowder was mixed with deionized water to form a slurry, and the slurry was ball-milled to obtain rare earth-doped YSZ agglomerates. The rare earth-doped YSZ agglomerates are subjected to at least two sintering processes to obtain intermediate powder; the sintering temperature of each sintering process is 900°C to 1300°C and the sintering time of each sintering process is 2h to 10h. The intermediate powder is sieved to obtain nano-agglomerated rare earth-doped YSZ powder.

2. The preparation method according to claim 1, characterized in that, Surface modification of a metal ion solution using a dispersant to obtain a reaction solution includes: The metal ion solution and dispersant are added to the impinging flow reactor containing deionized water; A precipitant is added dropwise to the impinging flow reactor, and a reaction solution is obtained by combining the stirring and ultrasonic operation of the impinging flow reactor. The precipitant is used to adjust the pH of the solution.

3. The preparation method according to claim 2, characterized in that, The precipitant is one or more of ammonium bicarbonate, ammonium hydroxide, and urea. The pH of the reaction solution is adjusted to between 8 and 11.

4. The preparation method according to claim 2, characterized in that, The stirring speed of the impinging flow reactor is 400 r / min to 2000 r / min, and the ultrasonic power is 10 kHz to 100 kHz.

5. The preparation method according to any one of claims 1 to 4, characterized in that, The zirconium salt is zirconium nitrate or zirconium dichloride, the yttrium salt is yttrium nitrate or yttrium chloride, and the rare earth salt includes gadolinium salt and / or ytterbium salt, wherein the gadolinium salt is gadolinium nitrate or gadolinium chloride, and the ytterbium salt is ytterbium nitrate or ytterbium chloride. The dispersant is one or a mixture of polyvinylpyrrolidone, hexadecyltrimethylammonium bromide, polyethylene glycol ethoxylates, and polyethylene glycol.

6. The preparation method according to claim 1, characterized in that, The process of sieving the intermediate powder includes: The intermediate powder is sieved using a sieve with a mesh size of 200 to 1000.

7. A nano-agglomerated rare earth-doped YSZ powder, characterized in that, The nano-agglomerated rare earth doped YSZ powder is prepared using the preparation method of nano-agglomerated rare earth doped YSZ powder according to any one of claims 1 to 6.

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