A method for preparing nanostructured YSZ target for EB-PVD

By combining nanostructured YSZ powder and spray granulation technology with cold isostatic pressing, the problem of target material fracture for EB-PVD coating under high-energy electron beam bombardment is solved, achieving efficient deposition and excellent thermal shock resistance, and being suitable for high-temperature environments.

CN119638415BActive Publication Date: 2025-09-23HARBIN INST OF TECH
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Patent Information

Application Number
CN202411992511.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-31
Publication Date
2025-09-23
Estimated Expiration
2044-12-31

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Abstract

The present invention discloses a preparation method of a nanostructured YSZ target for EB-PVD, the method comprising the following steps: one, proportioning nanostructured YSZ spherical powders of different particle sizes to obtain nanostructured YSZ spherical mixed powders of different particle sizes; two, adding deionized water to the YSZ spherical mixed powder, subsequently stirring the powder, paving and placing the aged powder to improve the forming performance, and obtaining the aged powder; three, pressing the aged powder using an upper and lower biaxial press, and the green body after demoulding is placed in a sealed bag and vacuumized; four, further pressing the green body after vacuum sealing using a cold isostatic pressing method to obtain a target green body; five, sintering the target green body to obtain a nanostructured YSZ target. The present invention can accurately control the target volume shrinkage by controlling the sintering route and particle size grading technology, simplifies the target preparation process flow, and reduces production costs.
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Description

Technical Field

[0001] The present invention relates to a method for preparing a target material for EB-PVD coating, and in particular to a method for preparing a nanostructured YSZ target material for EB-PVD. Background Art

[0002] Materials used for EB-PVD (electron beam physical vapor deposition) coatings must exhibit excellent heat resistance, given that they are deposited on areas of components that come into direct contact with high-temperature gases. Specifically, these materials must possess high melting points and high purity to ensure stability in extreme temperature environments. Furthermore, these coating materials must exhibit good adhesion to metal components, resist peeling during thermal cycling, resist corrosion by gas components, and possess low thermal conductivity to keep metal component temperatures as low as possible, thereby enhancing durability.

[0003] During the EB-PVD coating preparation process, when the target material (ingot) placed in the crucible is bombarded by a high-energy electron beam, if the vapor deposition material lacks the ability to adjust, it is very likely to fracture due to thermal shock. If such fracture occurs within the vapor deposition material, it will pose a significant obstacle to coating preparation, causing the target material to experience droplet splashing, cracking, and even shattering under stress and uneven microstructure. To improve the target material's thermal shock resistance, it is necessary to adjust its porosity. At the same time, the target material must also have better resistance to electron beam irradiation cracking. However, when the target material is made of large particles with a wide particle size distribution and poor shape uniformity, its microstructure is uneven. Therefore, during the vapor deposition process, when the target material is melted by electron beam irradiation, it is difficult to form a stable molten pool. In this case, the deposition efficiency is greatly reduced due to the uneven internal structure of the target material. Increasing the electron beam power to increase the deposition rate often leads to problems such as melt scattering. During the electron beam irradiation process, problems such as the rapid sintering of the material and the presence of internal porosity will accelerate the sintering process of the target material during rapid heating, making it unable to withstand the stress associated with sintering shrinkage and fracture, causing cracking. It is worth noting that cracks and pores have the function of absorbing thermal shock energy to a certain extent, which helps to improve the thermal shock resistance of the material. Therefore, by adjusting the microstructure of the internal material, its thermal shock resistance can be improved, thereby preventing stress-induced fracture. The sintered body is characterized by a porosity between 5% and 50%, and a pore volume range of 0.1 to 10 microns. In particular, pores in the range of 0.1 to 10 microns should account for more than 95% of the total pore volume. A porosity that is too low (less than 5%) will be detrimental to thermal shock resistance, because local heating during electron beam irradiation will generate thermal stress, which may lead to fracture. On the contrary, a porosity that is too high (over 50%) will reduce the mechanical strength of the sintered body and affect its operability. In addition, if the proportion of pores with a diameter of 0.1 to 10 microns is less than 90%, the thermal shock resistance of the sintered body will be insufficient, which is also not desirable. In the production process of vapor deposition materials, the green compacts usually need to undergo heat treatment. In order to improve the performance of the green compacts, it is recommended to carry out combustion treatment at 1100°C or higher. If the combustion temperature is low, the resulting vapor deposition material will undergo sintering and heating shrinkage during electron beam irradiation. This shrinkage will induce the generation of large-area stress, thereby increasing the risk of material cracking. Therefore, high-temperature combustion treatment helps to reduce sintering shrinkage during electron beam heating, thereby inhibiting the formation of cracks.

[0004] Nanoceramic materials developed using nanotechnology have microstructures with grains, grain boundaries, and their bonding all reaching the nanometer scale (1 to 100 nm). This characteristic significantly enhances the material's strength, toughness, and superplasticity, effectively overcoming the many shortcomings of traditional engineering ceramics. Simultaneously, it has a profound impact on key mechanical and thermal properties of the material, opening up new avenues for alternative applications in engineering ceramics. Nanoceramic powders, as nanoscale (0.1 to 100 nm) metastable transition states between solids and molecules, undergo ultrafine refinement, triggering unique changes in their surface electronic and crystal structures, exhibiting specific effects unmatched by bulk materials.

[0005] Specifically, nanopowder materials exhibit the following outstanding properties: their particle size is extremely small, their specific surface area is large, and they have excellent chemical properties. These properties can significantly reduce the sintering temperature of the material, thereby achieving effective energy conservation; at the same time, it can make the composition structure of the ceramic material denser and more uniform, significantly improving the performance of the ceramic material and enhancing its reliability. In addition, by precisely controlling the composition and structure of the material from the structural level of the nanomaterial (1 to 100nm), it is beneficial to fully explore and give full play to the potential advantages of ceramic materials. On the other hand, the particle size of ceramic powder has a decisive influence on the microstructure and macroscopic properties of ceramic materials. When the powder particles are evenly distributed, the shrinkage is consistent during the firing process, and the grains grow uniformly, the reduction in particle size will directly lead to a reduction in defects, thereby improving the strength of the prepared material. This characteristic makes it possible for nanopowder materials to exhibit some unique properties that are unmatched by traditional large-particle materials. Summary of the Invention

[0006] Based on the above considerations, the present invention provides a method for preparing a nanostructured YSZ target for EB-PVD. By utilizing fine nanostructured YSZ raw materials and combining them with spray granulation technology, this method not only successfully retains the properties of the nanostructure but also significantly improves the target's compressibility. Targets prepared from nanostructured raw materials exhibit high strength, excellent toughness, a stable internal structure, and uniform porosity. This reduces target firing time and improves target stability during use.

[0007] The object of the present invention is achieved through the following technical solutions:

[0008] A method for preparing a nanostructured YSZ target for EB-PVD comprises the following steps:

[0009] Step 1: Screen the nanostructured YSZ spherical powder according to the particle size, and mix the screened nanostructured YSZ spherical powders of different particle sizes according to the mass ratio to obtain nanostructured YSZ spherical mixed powders with different particle sizes, wherein:

[0010] The sieving specifications are 50-150 mesh, 150-300 mesh, 300-400 mesh, and the mass ratio is 2-6:1-3:1-5, and is used according to the powder particle size distribution and different porosity requirements;

[0011] The nanostructured YSZ spherical powder is one of nanostructured Y2O3 stabilized ZrO2 powder, rare earth doped Y2O3 stabilized ZrO2 powder, and enhanced phase doped Y2O3 stabilized ZrO2 powder, wherein the rare earth doping content is 1-20wt% and the enhanced phase content is 1-20wt%;

[0012] The nanostructured YSZ spherical powder is prepared by spray granulation technology, and the specific preparation steps are as follows:

[0013] Step (1) adding zirconium oxide grinding balls and an appropriate amount of deionized water to a vertical ball mill, then adding a certain amount of dispersant, adding ultrafine nanostructured YSZ powder after the dispersant is completely dissolved, and ball milling for a period of time, and then adding a certain amount of binder and continuing ball milling for a period of time to obtain a uniform slurry, wherein:

[0014] The particle size of the ultrafine nanostructured YSZ powder is 5 to 90 nm;

[0015] The ultra-fine nanostructured YSZ powder raw material is of 4N grade purity;

[0016] The ultrafine nanostructured YSZ powder is one of ultrafine grain structured Y2O3 stabilized ZrO2 powder, rare earth doped Y2O3 stabilized ZrO2 powder, and enhanced phase doped Y2O3 stabilized ZrO2 powder, wherein the rare earth doping content is 1-20wt% and the enhanced phase content is 1-20wt%;

[0017] The amount of deionized water used is 0.5 to 3 times the mass of the ultrafine nanostructured YSZ powder;

[0018] The dispersant is sodium tripolyphosphate (Na5P3O 10 ), sodium hexametaphosphate ((NaPO3)6), sodium pyrophosphate (Na4P2O7), ammonium citrate (C6H5O7(NH4)3), sodium citrate (C6H5Na3O7), polyvinyl alcohol (PVA), polyethylene glycol (PEG), etc. One or more of the dispersant, the amount of which is 0.03-6% of the mass of the ultrafine nanostructured YSZ powder;

[0019] The diameter of the zirconia grinding balls is 2 to 10 mm, the amount of zirconia grinding balls used is 1 to 5 times the mass of the ultrafine nanostructured YSZ powder, the total ball milling time is 6 to 24 hours, and the rotation speed is 300 to 1000 rpm;

[0020] The binder is one of gum arabic (Acacia), polyvinyl alcohol (PVA), carboxymethyl cellulose (CMC), tetraethyl orthosilicate (TEOS), etc., and the amount of the binder is 0.1 to 10% of the mass of the ultrafine nanostructured YSZ powder;

[0021] Step (2) The slurry obtained in step (1) is spray granulated to obtain micron-sized nanostructured spherical powder, and the powder is taken out and dried in an oven to obtain micron-sized nanostructured YSZ spherical powder, wherein:

[0022] The parameters of the spray granulation are as follows: the air inlet temperature is set at 200-250°C, the air outlet temperature is set at 100-130°C, the peristaltic pump speed is set at 30-45 r / min, and the needle passing speed is set at 10-15 t / min;

[0023] The drying temperature is 90-100°C and the drying time is 10-15h;

[0024] Step 2: Add deionized water to the YSZ spherical mixed powder obtained in step 1, then stir the powder, and lay the aged powder flat to improve the molding performance to obtain aged powder, wherein:

[0025] The amount of deionized water added is 3-8% of the mass of the YSZ spherical mixed powder;

[0026] The aging time of the powder is 5 to 10 hours;

[0027] Step 3: Stir the aged powder obtained in step 2 evenly, put it into a sleeve, and press it using an upper and lower biaxial press. After demoulding, the green body is put into a sealed bag and vacuumed, wherein:

[0028] The powder filling process uses ultrasonic vibration to improve density;

[0029] During the pressing process, the pressure is applied under upper and lower uniaxial pressure, the pressure is 20 to 50 MPa, and the pressure holding time is 10 to 30 minutes;

[0030] Step 4: The green body vacuum-sealed in step 3 is further pressed by cold isostatic pressing to obtain target green bodies with different porosities, wherein:

[0031] During the pressing process, the pressure is controlled at 150-250 MPa, and the holding time is controlled at 120-300 s.

[0032] The cold isostatic pressing method can use wet bag cold isostatic pressing, dry bag cold isostatic pressing, press pre-pressing and other molding methods. Preferably, the cold isostatic pressing method is wet bag cold isostatic pressing;

[0033] Step 5: Sintering the target material green body obtained in step 4 to obtain nanostructured YSZ targets with different porosities, wherein:

[0034] The sintering mechanism is as follows: first, the temperature is raised to 350°C (debinding temperature) at a rate of 1-5°C / min and kept for 300-420 minutes, then the temperature is raised to 800°C at a rate of 1-5°C / min and kept for 180-250 minutes, then the temperature is raised to 1150-1300°C (synthesis temperature) at a rate of 1-5°C / min and kept for 120-360 minutes, then the temperature is lowered to 600°C at a cooling rate of 1-5°C / min and kept for 120-150 minutes, and finally, the temperature is lowered to room temperature.

[0035] Compared with the prior art, the present invention has the following advantages:

[0036] 1. The present invention utilizes ultrafine nanostructured YSZ to prepare a nanostructured target suitable for electron beam physical vapor deposition, and provides a method for implementing the material on a thermal spray coating.

[0037] 2. The present invention is the first to use particle size adjustment technology and cold isostatic pressing process to prepare nanostructured target materials, which breaks through the problems of target materials easily cracking under high-energy electron beam bombardment, molten droplets easily splashing during the deposition process, and reduced deposition efficiency. The target materials prepared by the present invention have the advantages of high toughness, high strength, uniform internal structure, uniform pore distribution, wide material applicability, easy operation, high deposition efficiency, and easy industrialization.

[0038] 3. The present invention utilizes particle size classification and blending technology to press nanostructured spherical powder into a green body. In order to ensure that the overall volume shrinkage of the target material is minimized and a certain porosity is met, the target material sintering route is regulated to strictly control the porosity and volume shrinkage.

[0039] 4. This invention solves the problem of target material cracking and poor thermal shock resistance when suddenly bombarded by high-energy electron beams during use. The target material prepared by this invention has high toughness at high temperatures, excellent thermal shock resistance, and a stable internal structure, which has broad application prospects.

[0040] 5. The present invention can accurately control the volume shrinkage of the target material by controlling the sintering route and particle size grading technology, solving the problems of unstable size of the target material after sintering and the need for subsequent turning processing, simplifying the target material preparation process and reducing production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 This is the structure diagram of YSZ raw material before spray granulation;

[0042] Figure 2 This is the structure diagram of YSZ spherical agglomerates after spray granulation;

[0043] Figure 3 It is the green body of the target material after pressing;

[0044] Figure 4 The cross-sectional structure diagram of the target after sintering;

[0045] Figure 5 is the cross-sectional structure diagram of the target;

[0046] Figure 6 The pore distribution diagram. DETAILED DESCRIPTION

[0047] The technical solution of the present invention is further described below with reference to the embodiments, but is not limited thereto. Any modification or equivalent replacement of the technical solution of the present invention that does not depart from the spirit and scope of the technical solution of the present invention should be included in the scope of protection of the present invention.

[0048] Example 1:

[0049] This embodiment provides a method for preparing a nanostructured YSZ target for EB-PVD, the method comprising the following steps:

[0050] Step 1: ball-milling the nanostructured YSZ powder to prepare a slurry: adding zirconium oxide grinding balls and an appropriate amount of deionized water to a vertical ball mill, then adding a certain amount of dispersant, and after the dispersant is completely dissolved, adding the nanostructured YSZ powder and ball-milling for a period of time, adding a certain amount of binder and continuing ball-milling for a period of time to obtain a uniform slurry, wherein: the nanostructured YSZ powder is 4N grade purity and has a particle size of 20nm; the amount of the deionized water is twice the mass of the nanostructured YSZ powder; the dispersant is sodium hexametaphosphate ((NaPO3)6), and the amount of the dispersant is 1% of the mass of the nanostructured YSZ powder; the diameters of the zirconium oxide grinding balls are 3mm and 5mm, and the mass ratio is 6:4. The amount of the zirconium oxide grinding balls is twice the mass of the nanostructured YSZ powder. The ball milling time is 12h and the rotation speed is 600 rpm; the binder is gum arabic (Acacia), and the amount of the binder is 3% of the mass of the nanostructured YSZ powder.

[0051] Step 2: The slurry obtained in step 1 is spray granulated to obtain micron-sized spherical powder, wherein: the inlet air temperature is 245°C, the outlet air temperature is 120°C, the needle passing frequency is 10 times per minute, and the peristaltic pump rate is 40 revolutions per minute; the powder is taken out and dried in an oven at 90°C for 12 hours to obtain nanostructured YSZ powder.

[0052] Step 3: The nanostructured YSZ powder obtained in step 2 is sieved with three specifications of 150 mesh, 200 mesh, and 350 mesh, and the three specifications of powder obtained are mixed in a mass ratio of 5:3:2 to obtain nanostructured YSZ mixed powder.

[0053] Step 4: Add 5% deionized water to the nanostructured YSZ mixed powder obtained in step 3, then stir the powder, and lay the powder flat to age it for 10 hours to improve the molding performance, thereby obtaining aged powder.

[0054] Step 5: Stir the aged powder obtained in Step 4 evenly with a stainless steel spoon, place it in a stainless steel sleeve, and compact it using a biaxial press. Ultrasonic vibration is used during the powder filling process to increase density. Pressurize the powder under uniaxial pressure, controlling the pressure to 30 MPa and holding the pressure for 10 minutes. After demolding, place the green body in a sealed bag and evacuate it.

[0055] Step 6: The green body vacuum-sealed in step 5 is further pressed by a wet bag cold isostatic pressing method, with the pressure controlled at 200 MPa and the holding time controlled at 150 s to obtain a target green body.

[0056] Step 7: Use a box-type sintering furnace to sinter the target material green body obtained in step 6. The sintering mechanism is as follows: first, increase the temperature to 350°C (debinding temperature) at 2°C / min and keep it for 300 minutes, then increase it to 800°C at 2°C / min and keep it for 180 minutes, then increase it to 1200°C (synthesis temperature) at 2°C / min and keep it for 120 minutes, then cool it to 600°C at a cooling rate of 2°C / min and keep it for 180 minutes, finally, cool the temperature to room temperature to obtain a nanostructured YSZ target.

[0057] In this embodiment, the structure of YSZ raw material before spray granulation is as follows: Figure 1 As shown, the structure of YSZ spherical agglomerates after spray granulation is as follows Figure 2 As shown in the figure, the spherical shape is good after spray granulation, and the spherical diameter distribution is uniform. Figure 3 As shown in the figure, the target material has a diameter of 80 mm and a height of 100 mm before sintering. The cross-sectional structure of the target material after sintering is as follows: Figure 4 As shown, the cross-sectional structure of the target is as follows Figure 5 As shown, the pore distribution is Figure 6 As shown. Figure 1 It can be seen that the original grains of YSZ raw materials conform to the nanostructure; Figure 4 It can be seen that the grains of the nanostructured YSZ target are small and uniform, and the grain size distribution is between 100 and 500 nm. Figure 5 and Figure 6 It can be seen that the pore distribution of the nanostructured YSZ target is uniform, the pore size is uniform, and there are no obvious defects; the density and volume shrinkage of the target are shown in Table 1.

[0058] Table 1

[0059]

[0060] Example 2:

[0061] This embodiment provides a method for preparing a nanostructured CeO2-doped YSZ target for EB-PVD, the method comprising the following steps:

[0062] Step 1: Mix the nanostructured YSZ powder and the nanostructured CeO2 and then ball-mill to prepare a slurry: add zirconium oxide grinding balls and an appropriate amount of deionized water into a vertical ball mill, then add a certain amount of dispersant, and after the dispersant is completely dissolved, add the nanostructured CeO2 and the nanostructured YSZ powder and ball-mill for a period of time, then add a certain amount of binder and continue ball-milling for a period of time to obtain a uniform slurry, wherein: the nanostructured YSZ powder is 4N grade purity and has a particle size of 5 to 90 nm; the nanostructured CeO2 powder is 4N grade purity and has a particle size of 2 0nm, and the added amount is 3wt% of the mixed powder mass; the amount of deionized water is 3 times the mass of the mixed powder; the dispersant is sodium hexametaphosphate ((NaPO3)6, and the amount of the dispersant is 1.5% of the mass of the mixed powder; the diameters of the zirconia grinding balls are 3mm and 5mm, the mass ratio is 6:4, the amount of the zirconia grinding balls is 2 times the mass of the nanostructured YSZ powder, the ball milling time is 12h, and the number of revolutions is 800 rpm; the binder is polyvinyl alcohol (PVA), and the amount of the binder is 1.5% of the mass of the mixed powder.

[0063] Step 2: The slurry obtained in step 1 is spray granulated to obtain micron-scale spherical powder, wherein: the inlet air temperature is 220°C, the outlet air temperature is 100°C, the needle passing frequency is 15 times per minute, and the peristaltic pump rate is 35 revolutions per minute; the powder is taken out and dried in an oven at 90°C for 12 hours to obtain CeO2-doped nanostructured YSZ agglomerated powder.

[0064] Step 3: The CeO2-doped nanostructured YSZ agglomerated powder obtained in step 2 is sieved with three specifications of 100 mesh, 200 mesh, and 400 mesh, and the three specifications of powder obtained are mixed in a mass ratio of 6:2:2 to obtain CeO2-doped nanostructured YSZ agglomerated mixed powder.

[0065] Step 4: Add 5% deionized water to the CeO2-doped nanostructured YSZ agglomerated mixed powder obtained in step 3, then stir the powder, and lay the powder flat to age for 6 hours to improve the molding performance, thereby obtaining aged powder.

[0066] Step 5: Stir the aged powder obtained in Step 4 evenly with a stainless steel spoon, place it in a stainless steel sleeve, and compact it using a biaxial press. Ultrasonic vibration is used during the powder filling process to increase density. Pressurize the powder under uniaxial pressure, controlling the pressure to 30 MPa and holding the pressure for 10 minutes. After demolding, place the green body in a sealed bag and evacuate it.

[0067] Step 6: The green body vacuum-sealed in step 5 is further pressed by a wet bag cold isostatic pressing method, with the pressure controlled at 200 MPa and the holding time controlled at 150 s to obtain a target green body.

[0068] Step 7: The target green body obtained in Step 6 was sintered in a box-type sintering furnace. The sintering mechanism was as follows: first, the temperature was raised to 350°C (debinding temperature) at a rate of 2°C / min and held for 300 minutes. Then, the temperature was raised to 800°C at a rate of 2°C / min and held for 250 minutes. Subsequently, the temperature was raised to 1200°C (synthesis temperature) at a rate of 2°C / min and held for 360 minutes. Subsequently, the temperature was lowered to 600°C at a rate of 2°C / min and held for 120 minutes. Finally, the temperature was lowered to room temperature to obtain a nanostructured CeO2-doped nanostructured YSZ agglomerated powder target. The target density and volume shrinkage are shown in Table 1.

Claims

1. A method for preparing a nanostructured YSZ target for EB-PVD, characterized in that The method comprises the following steps: Step 1: Screening the nanostructured YSZ spherical powder according to the particle size, and mixing the screened nanostructured YSZ spherical powders of different particle sizes according to the mass ratio to obtain nanostructured YSZ spherical mixed powders with different particle sizes, wherein: the screening specifications are 50-150 mesh, 150-300 mesh, and 300-400 mesh, and the mass ratio is 2-6:1-3:1-5, and the powders are used according to the particle size distribution and different porosity requirements of the powders; the nanostructured YSZ spherical powder is prepared by spray granulation technology; Step 2: adding deionized water to the YSZ spherical mixed powder obtained in step 1, stirring the powder, and laying out the aged powder to improve the molding performance to obtain aged powder; Step 3: Stir the aged powder obtained in step 2 evenly, put it into a sleeve, and press it using an upper and lower biaxial press. After demoulding, put the green embryo into a sealed bag and vacuum it; Step 4: further pressing the green embryo vacuum-sealed in step 3 by cold isostatic pressing to obtain target green embryos with different porosities; Step 5. Sinter the target material green body obtained in step 4 to obtain a nanostructured YSZ target with different porosities, wherein: the sintering mechanism is: first, increase the temperature to 350°C at a rate of 1~5°C / min and keep it for 300~420min, then increase the temperature to 800°C at a rate of 1~5°C / min and keep it for 180~250min, then increase the temperature to 1150~1300°C at a rate of 1~5°C / min and keep it for 120~360min, then reduce the temperature to 600°C at a cooling rate of 1~5°C / min and keep it for 120~150min, and finally reduce the temperature to room temperature.

2. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 1, characterized in that The nanostructured YSZ spherical powder is one of nanostructured Y2O3 stabilized ZrO2 powder, rare earth doped Y2O3 stabilized ZrO2 powder, and enhanced phase doped Y2O3 stabilized ZrO2 powder, with a rare earth doping content of 1-20wt% and an enhanced phase content of 1-20wt%.

3. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 1 or 2, characterized in that The specific preparation steps of the nanostructured YSZ spherical powder are as follows: Step (1): adding zirconium oxide grinding balls and deionized water to a vertical ball mill, then adding a dispersant, and after the dispersant is completely dissolved, adding ultrafine nanostructured YSZ powder and ball milling for a period of time, adding a binder and continuing ball milling for a period of time to obtain a uniform slurry, wherein: the amount of deionized water is 0.5 to 3 times the mass of the ultrafine nanostructured YSZ powder, the amount of the dispersant is 0.03 to 6% of the mass of the ultrafine nanostructured YSZ powder, and the amount of the binder is 0.1 to 10% of the mass of the ultrafine nanostructured YSZ powder; Step (2): The slurry obtained in step (1) is spray granulated to obtain micron-sized nanostructured spherical powder, and the powder is taken out and dried in an oven to obtain micron-sized nanostructured YSZ spherical powder.

4. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 3, characterized in that The dispersant is one or more of sodium tripolyphosphate, sodium hexametaphosphate, sodium pyrophosphate, ammonium citrate, sodium citrate, polyvinyl alcohol, and polyethylene glycol; the diameter of the zirconia grinding balls is 2 to 10 mm; the amount of the zirconia grinding balls is 1 to 5 times the mass of the ultrafine nanostructured YSZ powder; the total ball milling time is 6 to 24 hours, and the number of revolutions is 300 to 1000 revolutions per minute; and the binder is one of gum arabic, polyvinyl alcohol, carboxymethyl cellulose, and ethyl silicate.

5. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 3, characterized in that The parameters of the spray granulation are as follows: the air inlet temperature is set at 200-250°C, the air outlet temperature is set at 100-130°C, the peristaltic pump speed is set at 30-45 r / min, and the needle passing speed is set at 10-15 t / min.

6. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 3, characterized in that The drying temperature is 90-100° C., and the drying time is 10-15 hours.

7. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 1, characterized in that The aging time of the powder is 5 to 10 hours.

8. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 1, characterized in that When the upper and lower biaxial presses are used for pressing, the pressing is performed under upper and lower uniaxial pressures, the pressure is 20-50 MPa, and the holding time is 10-30 minutes.

9. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 1, characterized in that When the cold isostatic pressing method is used for pressing, the pressure is controlled at 150-250 MPa, and the holding time is controlled at 120-300 s.

10. The method for preparing a nanostructured YSZ target for EB-PVD according to claim 1 or 9, characterized in that The cold isostatic pressing method uses a wet bag cold isostatic pressing, a dry bag cold isostatic pressing, and a press pre-pressing molding method.

Citation Information

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