A method for preparing a single tetragonal phase zirconia stable at high temperature, ultrahigh temperature
By using water-soluble inorganic salts and chelating agents to prepare zirconia precursors under non-strong alkaline conditions and calcining them at high temperatures, the problems of complex equipment and environmental pollution in existing technologies are solved, enabling efficient and environmentally friendly large-scale production of high-temperature stable single tetragonal phase zirconia.
Patent Information
- Application Number
- CN202410600391.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-15
- Publication Date
- 2026-02-03
- Estimated Expiration
- 2044-05-15
AI Technical Summary
Existing technologies for preparing high-performance single tetragonal zirconia involve complex equipment, environmental pollution from the use of organic reagents, and high costs, making it difficult to achieve stable mass production.
Zirconia precursors were prepared by a one-step water bath method under non-strong alkaline conditions using water-soluble inorganic zirconium salts and yttrium salts, combined with food-grade metal ion chelating agents. Subsequently, stable single tetragonal phase zirconia was obtained by high-temperature and ultra-high-temperature calcination in air.
This technology enables large-scale, environmentally friendly, and low-cost production of high-temperature and ultra-high-temperature stable single tetragonal phase zirconia, simplifying the process, improving the stability and crystallinity of the material, and making it suitable for commercial applications.
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Figure CN118324181B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of ceramic nanomaterials technology, specifically relating to a method for preparing a single tetragonal phase zirconia that is stable at high and ultra-high temperatures. Background Technology
[0002] Zirconia ceramics possess chemical stability and biocompatibility. Furthermore, compared to other ceramic materials, they exhibit high strength and toughness. Zirconia-based materials are widely used in aerospace, chemical, medical, electronics, and energy fields. With the diversification of zirconia ceramic materials, higher requirements are being placed on the purity and stability of the ceramic powder phase.
[0003] Normally, zirconium oxide exists only as a monoclinic phase at room temperature, but it can interconvert into three crystal forms within different temperature ranges: monoclinic (m-ZrO2), tetragonal (t-ZrO2), and cubic (c-ZrO2). Tetragonal zirconium oxide, as a thermal barrier coating, exhibits excellent resistance to thermal cycling and thermal shock. Its mechanical properties are superior to cubic zirconium oxide, making it suitable as a reinforcing and toughening phase in self-cleaning films and as a matrix phase in denture restoration. Chinese patent CN116282145 A discloses a method for preparing high-purity tetragonal zirconium oxide nanoparticles using supercritical hydrothermal synthesis equipment under alkaline conditions through a hydrothermal metathesis reaction. However, this method involves complex equipment, some XRD patterns show unclear tetragonal phase peaks, and the use of alkaline reagents can cause environmental pollution. Chinese patent CN 117282398A discloses a method for preparing an amine-functionalized porous MgO / ZrO2 composite adsorbent. In this method, an organic zirconium source is added, and solvent evaporation leads to self-assembly to form a zirconium-containing wet gel, which is then sintered at high temperature to produce zirconium oxide material. However, the organic zirconium source used in this method is expensive, and the use of organic reagents can cause environmental pollution.
[0004] Therefore, in the industrialization process of high-performance single tetragonal zirconia, improving the stability of zirconia and achieving stable mass production is particularly important. Summary of the Invention
[0005] To address the shortcomings of existing technologies, this invention provides a method for preparing single tetragonal zirconia that is stable at high and ultra-high temperatures. This method is simple, easy to implement, and suitable for large-scale production.
[0006] The present invention adopts the following technical solution:
[0007] A method for preparing single tetragonal phase zirconia stable at high and ultra-high temperatures specifically includes the following steps:
[0008] Step 1: Prepare zirconium salt solution. Weigh ZrOCl2 into a beaker, add deionized water, and stir until completely dissolved to obtain zirconium salt solution.
[0009] Step 2: Prepare yttrium salt solution. Weigh Y(NO3)3 into a beaker, add deionized water and stir until homogeneous to obtain yttrium salt solution.
[0010] Step 3: Prepare the chelating agent solution by weighing C4H6O6, C6H8O7, C2H2O4, C2H7NO, and C... 10 H 14 N2Na2O8 or C 10 H 12 One of N2Na4O8 is added to deionized water and stirred until completely dissolved to obtain a chelating agent solution;
[0011] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, stir evenly, and the resulting white turbid liquid is the zirconium oxide precursor solution;
[0012] Step 5: Place the zirconia precursor solution obtained in step 4 into a water bath for reaction, centrifuge and wash, and then dry in an oven to obtain a single tetragonal phase zirconia precursor powder.
[0013] Step 6: Place the single tetragonal zirconia precursor powder obtained in Step 5 into a muffle furnace and calcine it in air at high and ultra-high temperatures to obtain the single tetragonal zirconia material.
[0014] Furthermore, in step 1, the mass of ZrOCl2 is 16.0-64.0g, and the amount of deionized water is 50-200mL.
[0015] Furthermore, in step 2, the mass of Y(NO3)3 is 1.2-4.8g, and the amount of deionized water is 25-100mL.
[0016] Furthermore, in step 3, C4H6O6, C6H8O7, C2H2O4, C2H7NO, and C 10 H 14 N2Na2O8 or C 10 H 12 The mass of N2Na4O8 is 7.4-55.4g, and the mass of deionized water is 50-200mL.
[0017] Furthermore, the stirring process in steps 1-4 is carried out using a magnetic stirrer, and the stirring time is 10-60 minutes.
[0018] Furthermore, step 4, preparing the zirconium oxide precursor solution, is carried out under non-strongly alkaline conditions.
[0019] Furthermore, in step 5, the water bath temperature is 60-80℃, the water bath time is 2-6 hours, and the washing method is as follows: first wash with deionized water three times, then wash with anhydrous ethanol three times, and dry in an oven at 60℃ for 24-36 hours.
[0020] Furthermore, the calcination temperature in step 6 is 400-1300℃, and the holding time is 1-2 hours.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] (1) The zirconium salts and yttrium salts used in this invention are both water-soluble inorganic salts, and do not require volatile or toxic organic reagents for dissolution, making them more environmentally friendly. Compared to organometallic zirconium salts such as zirconium ethoxide (C8H4O2), these are more environmentally friendly. 20 O4Zr), zirconium tert-butoxide (C4H) 10 OZr), zirconium propoxide (C) 12 H 28 The price of zirconium salts is several times lower than that of organic zirconium salts, and the conditions for their use are quite demanding, generally requiring reaction in organic reagents, which increases the complexity of the process and environmental pollution. Therefore, the zirconium salts and yttrium salts used in this invention are inexpensive, readily available, and environmentally friendly.
[0023] (2) The metal ion chelating agents used in this invention include: tartaric acid (C4H6O6), citric acid (C6H8O7), oxalic acid (C2H2O4), ethanolamine (C2H7NO), and disodium ethylenediaminetetraacetate (C4H6O6). 10 H 14 N2Na2O8) or tetrasodium ethylenediaminetetraacetate (C 10 H 12 Using metal ion chelating agents (N2Na4O8) has two advantages: first, the selected reagents are all food-grade additives, ensuring biological safety; second, the addition of the chelating agent utilizes its interaction with metal ions (Zr). 4+ A reaction can occur to generate a stable chelate precursor, and further post-processing can achieve the preparation of a single tetragonal zirconium oxide without the need for strong base reagents.
[0024] (3) The preparation process of this invention is simple. The product can be obtained by one-pot method and one-step water bath. It is simple, easy to carry out and has good repeatability. The synthesized product has high performance and good stability. It is suitable for large-scale production and can promote the commercialization of high-performance ceramic materials.
[0025] (4) The products prepared by this invention can be single tetragonal zirconium oxide after high temperature and ultra-high temperature calcination, and can be stable tetragonal phase in the high temperature and ultra-high temperature range. Attached Figure Description
[0026] Figure 1This is a flowchart of a method for preparing a single tetragonal phase zirconia that is stable at high and ultra-high temperatures according to the present invention.
[0027] Figure 2 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 1 of this invention;
[0028] Figure 3 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 2 of this invention;
[0029] Figure 4 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 3 of this invention;
[0030] Figure 5 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 4 of this invention;
[0031] Figure 6 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 5 of this invention;
[0032] Figure 7 The image shows the XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 6 of this invention. Detailed Implementation
[0033] like Figure 1 As shown, a method for preparing single tetragonal zirconia stable at high and ultra-high temperatures specifically includes the following steps:
[0034] Step 1: Prepare zirconium salt solution. Weigh 16.0-64.0g ZrOCl2 into a beaker, add 50-200mL of deionized water, and stir until completely dissolved to obtain zirconium salt solution.
[0035] Step 2: Prepare yttrium salt solution. Weigh 1.2-4.8g of Y(NO3)3 into a beaker, add 25-100mL of deionized water and stir well to obtain yttrium salt solution.
[0036] Step 3: Prepare the chelating agent solution by weighing 7.4-55.4g of C4H6O6, C6H8O6, C2H2O4, C2H7NO, and C... 10 H 14 N2Na2O8 or C 10 H 12 Add N2Na4O8 and 50-200mL of deionized water, and stir until completely dissolved to obtain a chelating agent solution;
[0037] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, stir evenly, and the resulting white turbid liquid is the zirconium oxide precursor solution. The preparation of the zirconium oxide precursor solution is carried out under non-strong alkaline conditions.
[0038] Step 5: Prepare zirconia precursor powder in a water bath. Place the precursor solution in a water bath and react at a temperature of 60-80℃ for 2-6 hours. After centrifugation and washing, place it in an oven to dry. The washing method is as follows: wash three times with deionized water and then three times with anhydrous ethanol. Dry in an oven at 60℃ for 24-36 hours to obtain a single tetragonal phase zirconia precursor powder.
[0039] Step 6, High-temperature and ultra-high-temperature sintering to prepare single tetragonal phase zirconia material: The precursor powder obtained in step 5 is placed in a muffle furnace and calcined in air at high and ultra-high temperatures of 400-1300℃ for 1-2 hours to obtain single tetragonal phase zirconia that is stable in the high-temperature and ultra-high-temperature range.
[0040] Example 1
[0041] Step 1, prepare zirconium salt solution: Weigh 16.0g ZrOCl2 into a beaker, add 50mL deionized water, and stir with a magnetic stirrer for 10min to obtain zirconium salt solution;
[0042] Step 2, prepare yttrium salt solution: Weigh 1.2g Y(NO3)3 into a beaker, add 25mL of deionized water and stir well. Stir with a magnetic stirrer for 10min to obtain yttrium salt solution;
[0043] Step 3, prepare chelating agent solution: Weigh 18.3g C4H6O6 into a beaker, add 50mL of deionized water, and stir with a magnetic stirrer for 10min to obtain chelating agent solution;
[0044] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, and stir with a magnetic stirrer for 10 minutes. The resulting white turbid liquid is the zirconium oxide precursor solution.
[0045] Step 5, water bath preparation of precursor powder: Place the zirconia precursor solution obtained in step 4 into a water bath and bathe it at 80℃ for 4 hours; when centrifuging and washing, first wash it three times with deionized water, then wash it three times with anhydrous ethanol; finally, dry it in an oven at 60℃ for 24 hours to obtain zirconia precursor powder.
[0046] Step 6, High-temperature sintering to prepare zirconia nanomaterials: The zirconia precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at 800℃ for 2 hours to obtain single tetragonal zirconia nanoparticles.
[0047] like Figure 2The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 1 of this invention is shown. It is in perfect agreement with the standard card of tetragonal zirconia (JCPDS NO.88-1007). The prepared zirconia nanomaterial has good crystallinity and no impurity phase. The c / a value is calculated to be 1.435 from the pattern. The grain size is calculated to be 23.8 nm using the Scherrer equation.
[0048] Example 2
[0049] Step 1, prepare zirconium salt solution: Weigh 26.0g ZrOCl2 into a beaker, add 100mL deionized water, and stir with a magnetic stirrer for 30min to obtain zirconium salt solution;
[0050] Step 2, prepare yttrium salt solution: Weigh 2.4g Y(NO3)3 into a beaker, add 50mL of deionized water and stir well. Stir with a magnetic stirrer for 30min to obtain yttrium salt solution;
[0051] Step 3, prepare chelating agent solution: Weigh 36.6g C6H8O7 into a beaker, add 100mL deionized water, and stir with a magnetic stirrer for 30min to obtain chelating agent solution;
[0052] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, and stir with a magnetic stirrer for 30 minutes. The resulting white turbid liquid is the zirconium oxide precursor solution.
[0053] Step 5, water bath preparation of precursor powder: The zirconia precursor solution obtained in step 4 is placed in a water bath and heated at 60°C for 6 hours; during centrifugation and washing, it is first washed three times with deionized water and then three times with anhydrous ethanol; finally, it is dried in a 60°C oven for 30 hours to obtain zirconia precursor powder.
[0054] Step 6, ultra-high temperature sintering to prepare zirconia nanomaterials: The zirconia precursor powder obtained in step 5 is placed in a muffle furnace and calcined at an ultra-high temperature of 1300℃ in air for 1 hour to obtain single tetragonal phase zirconia nanoparticles.
[0055] like Figure 3 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 2 of this invention is shown. It is in perfect agreement with the standard card of tetragonal zirconia (JCPDS NO.88-1007). The prepared zirconia nanomaterial has good crystallinity and no impurity phase. The c / a value is calculated to be 1.435 from the spectrum. The grain size is calculated to be 38.0 nm using the Scherrer equation.
[0056] Example 3
[0057] Step 1, prepare zirconium salt solution: Weigh 64.0g ZrOCl2 into a beaker, add 200mL deionized water, and stir with a magnetic stirrer for 60min to obtain zirconium salt solution;
[0058] Step 2, prepare yttrium salt solution: Weigh 4.8g Y(NO3)3 into a beaker, add 100mL deionized water and stir well. Stir with a magnetic stirrer for 60min to obtain yttrium salt solution;
[0059] Step 3, prepare the chelating agent solution: Weigh 15.3g C2H2O4 into a beaker, add 100mL of deionized water, and stir with a magnetic stirrer for 60min to obtain the chelating agent solution;
[0060] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, and stir with a magnetic stirrer for 60 minutes. The resulting white turbid liquid is the zirconium oxide precursor solution.
[0061] Step 5, water bath preparation of precursor powder: The zirconia precursor solution obtained in step 4 is placed in a water bath and heated at 70°C for 6 hours; during centrifugation and washing, it is first washed three times with deionized water and then three times with anhydrous ethanol; finally, it is dried in an oven at 60°C for 36 hours to obtain zirconia precursor powder.
[0062] Step 6, High-temperature sintering to prepare zirconia nanomaterials: The zirconia precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at 600℃ for 2 hours to obtain single tetragonal zirconia nanoparticles.
[0063] like Figure 4 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 3 of this invention is shown. It is in perfect agreement with the standard card of tetragonal zirconia (JCPDS NO.88-1007). The prepared zirconia nanomaterial has good crystallinity and no impurity phase. The c / a value is calculated to be 1.426 from the spectrum. The grain size is calculated to be 17.1 nm using the Scherrer equation.
[0064] Example 4
[0065] Step 1, prepare zirconium salt solution: Weigh 16.0g ZrOCl2 into a beaker, add 50mL deionized water, and stir with a magnetic stirrer for 10min to obtain zirconium salt solution;
[0066] Step 2, prepare yttrium salt solution: Weigh 1.2g Y(NO3)3 into a beaker, add 25mL of deionized water and stir well. Stir with a magnetic stirrer for 10min to obtain yttrium salt solution;
[0067] Step 3, prepare the chelating agent solution: Weigh 55.4g of C 10 H 14 Place N2Na2O8 in a beaker, add 200mL of deionized water, and stir with a magnetic stirrer for 10 minutes to obtain a chelating agent solution;
[0068] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, and stir with a magnetic stirrer for 30 minutes. The resulting white turbid liquid is the zirconium oxide precursor solution.
[0069] Step 5, water bath preparation of precursor powder: Place the zirconia precursor solution obtained in step 4 into a water bath and bathe it at 60°C for 6 hours; wash it three times with deionized water and then three times with anhydrous ethanol during centrifugation; finally, dry it in an oven at 60°C for 24 hours to obtain zirconia precursor powder.
[0070] Step 6, ultra-high temperature sintering to prepare zirconia nanomaterials: The zirconia precursor powder obtained in step 5 is placed in a muffle furnace and calcined at an ultra-high temperature of 1300℃ in air for 1.5h to obtain single tetragonal zirconia nanoparticles.
[0071] like Figure 5 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 4 of this invention is shown. It is in perfect agreement with the standard card of tetragonal zirconia (JCPDS NO.88-1007). The prepared zirconia nanomaterial has good crystallinity and no impurity phase. The c / a value is calculated to be 1.435 from the spectrum. The grain size is calculated to be 37.2 nm using the Scherrer equation.
[0072] Example 5
[0073] Step 1, prepare zirconium salt solution: Weigh 16.0g ZrOCl2 into a beaker, add 50mL deionized water, and stir with a magnetic stirrer for 10min to obtain zirconium salt solution;
[0074] Step 2, prepare yttrium salt solution: Weigh 1.2g Y(NO3)3 into a beaker, add 25mL of deionized water and stir well. Stir with a magnetic stirrer for 10min to obtain yttrium salt solution;
[0075] Step 3, prepare chelating agent solution: Weigh 7.4g C2H7NO into a beaker, add 50mL deionized water, and stir with a magnetic stirrer for 10min to obtain chelating agent solution;
[0076] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, and stir with a magnetic stirrer for 30 minutes. The resulting white turbid liquid is the zirconium oxide precursor solution.
[0077] Step 5, water bath preparation of precursor powder: Place the zirconia precursor solution obtained in step 4 into a water bath and bathe it at 80°C for 2 hours; when centrifuging and washing, first wash it three times with deionized water, then wash it three times with anhydrous ethanol; finally, dry it in an oven at 60°C for 24 hours to obtain zirconia precursor powder.
[0078] Step 6, ultra-high temperature sintering to prepare zirconia nanomaterials: The zirconia precursor powder obtained in step 5 is placed in a muffle furnace and calcined at an ultra-high temperature of 800℃ in air for 2 hours to obtain single tetragonal phase zirconia nanoparticles.
[0079] like Figure 6 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 5 of this invention is shown. It is in perfect agreement with the standard card of tetragonal zirconia (JCPDS NO.88-1007). The prepared zirconia nanomaterial has good crystallinity and no impurity phase. The c / a value is calculated to be 1.431 from the spectrum. The grain size is calculated to be 16.6 nm using the Scherrer equation.
[0080] Example 6
[0081] Step 1, prepare zirconium salt solution: Weigh 16.0g ZrOCl2 into a beaker, add 50mL deionized water, and stir with a magnetic stirrer for 10min to obtain zirconium salt solution;
[0082] Step 2, prepare yttrium salt solution: Weigh 1.2g Y(NO3)3 into a beaker, add 25mL of deionized water and stir well. Stir with a magnetic stirrer for 10min to obtain yttrium salt solution;
[0083] Step 3, prepare the chelating agent solution: Weigh 7.4g C 10 H 12 Place N2Na4O8 in a beaker, add 50mL of deionized water, and stir with a magnetic stirrer for 10min to obtain a chelating agent solution;
[0084] Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, and stir with a magnetic stirrer for 30 minutes. The resulting white turbid liquid is the zirconium oxide precursor solution.
[0085] Step 5, water bath preparation of precursor powder: Place the zirconia precursor solution obtained in step 4 into a water bath and bathe it at 80℃ for 4 hours; when centrifuging and washing, first wash it three times with deionized water, then wash it three times with anhydrous ethanol; finally, dry it in an oven at 60℃ for 24 hours to obtain zirconia precursor powder.
[0086] Step 6, ultra-high temperature sintering to prepare zirconia nanomaterials: The zirconia precursor powder obtained in step 5 is placed in a muffle furnace and calcined at an ultra-high temperature of 1300℃ in air for 2 hours to obtain single tetragonal zirconia nanoparticles.
[0087] like Figure 7 The XRD pattern of the tetragonal zirconia nanoparticles obtained in Example 6 of this invention is shown. It is in perfect agreement with the standard card of tetragonal zirconia (JCPDS NO.88-1007). The prepared zirconia nanomaterial has good crystallinity and no impurity phase. The c / a value is calculated to be 1.436 from the spectrum. The grain size is calculated to be 33.9 nm using the Scherrer equation.
[0088] While specific embodiments of the present invention have been described above, those skilled in the art should understand that these are merely illustrative examples, and the scope of protection of the present invention is defined by the appended claims. Those skilled in the art can make various changes or modifications to these embodiments without departing from the principles and essence of the present invention, but all such changes and modifications fall within the scope of protection of the present invention.
Claims
1. A method for preparing single tetragonal phase zirconia stable at high and ultra-high temperatures, characterized in that, Specifically, the following steps are included: Step 1: Prepare zirconium salt solution. Weigh ZrOCl2 into a beaker, add deionized water, and stir until completely dissolved to obtain zirconium salt solution. Step 2: Prepare yttrium salt solution. Weigh Y(NO3)3 into a beaker, add deionized water and stir until homogeneous to obtain yttrium salt solution. Step 3: Prepare the chelating agent solution by weighing C4H6O6, C6H8O7, C2H2O4, C2H7NO, and C... 10 H 14 N2Na2O8 or C 10 H 12 One of N2Na4O8 is added to deionized water and stirred until completely dissolved to obtain a chelating agent solution; Step 4: Add the yttrium salt solution and chelating agent solution obtained in Step 2 and Step 3 to the zirconium salt solution obtained in Step 1 in sequence, stir evenly, and the resulting white turbid liquid is the zirconium oxide precursor solution; Step 5: Place the zirconia precursor solution obtained in step 4 into a water bath for reaction, centrifuge and wash, and then dry in an oven to obtain a single tetragonal phase zirconia precursor powder. Step 6: Place the single tetragonal zirconia precursor powder obtained in Step 5 into a muffle furnace and calcine it in air at high and ultra-high temperatures to obtain the single tetragonal zirconia material.
2. The method for preparing a single tetragonal phase zirconia stabilized at high and ultra-high temperatures according to claim 1, characterized in that, In step 1, the mass of ZrOCl2 is 16.0-64.0g, and the amount of deionized water is 50-200mL.
3. The method for preparing a single tetragonal phase zirconia stabilized at high and ultra-high temperatures according to claim 1, characterized in that, In step 2, the mass of Y(NO3)3 is 1.2-4.8g, and the amount of deionized water is 25-100mL.
4. The method for preparing a single tetragonal phase zirconia stabilized at high and ultra-high temperatures according to claim 1, characterized in that, In step 3, C4H6O6, C6H8O7, C2H2O4, C2H7NO, and C 10 H 14 N2Na2O8 or C 10 H 12 The mass of N2Na4O8 is 7.4-55.4g, and the mass of deionized water is 50-200mL.
5. The method for preparing a single tetragonal phase zirconia stabilized at high and ultra-high temperatures according to claim 1, characterized in that, The stirring process in steps 1-4 is carried out using a magnetic stirrer, and the stirring time is 10-60 minutes.
6. The method for preparing a single tetragonal phase zirconia stabilized at high and ultra-high temperatures according to claim 1, characterized in that, Step 4, preparing the zirconium oxide precursor solution, is carried out under non-strongly alkaline conditions.
7. The method for preparing a single tetragonal phase zirconia stabilized at high and ultra-high temperatures according to claim 1, characterized in that, In step 5, the water bath temperature is 60-80℃, the water bath time is 2-6 hours, and the washing method is as follows: first wash with deionized water three times, then wash with anhydrous ethanol three times, and dry in an oven at 60℃ for 24-36 hours.
8. The method for stabilizing single tetragonal phase zirconia at high and ultra-high temperatures according to claim 1, characterized in that, The calcination temperature in step 6 is 400-1300℃, and the holding time is 1-2 hours.
Citation Information
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