A method for preparing nano-yttrium oxide based on the double-cage effect

Abstract

This invention discloses a method for preparing nano-yttrium oxide based on the double-cage effect. The method uses Y(NO3)3·6H2O or YCl3·6H2O as the yttrium salt, and C4H6O6 as a "cage" as a chelating agent to directly chelate with metal ions, thus encapsulating the metallic Y in a cage-like structure. 3+ By using syrup as an auxiliary agent to graft onto the outside of a chelating agent to form a "double cage," the growth of crystal nuclei is stabilized, and the uniform nucleation of yttrium oxide is regulated by the double-cage structure. Under high-concentration acidic conditions, the crystal growth rate is controlled by a water bath reaction, and nano-yttrium oxide materials are successfully prepared. The synthesis process of this invention uses inexpensive and readily available inorganic salts and food-grade additives as raw materials, which is not only low-cost but also environmentally friendly and safe. It conforms to the green technology innovation advocated by the "dual carbon" strategy. It is simple, easy to implement, and has good reproducibility, which can be mass-produced and can effectively promote the commercialization of functional ceramic materials.

Description

Technical Field

[0001] This invention belongs to the field of ceramic materials technology, specifically relating to a method for preparing nano-yttrium oxide based on the double-cage effect. Background Technology

[0002] Nanoceramic powders are substances with nanoscale dimensions, falling between solids and molecules. Nanoparticle materials possess extremely small particle sizes, large specific surface areas, and high chemical properties, which can significantly reduce sintering temperatures and save energy. Nanoscale powders are beneficial for improving the density and mechanical properties of ceramic materials. Furthermore, due to their small particle size, if the grains grow uniformly during firing, they may exhibit unique properties not found in larger particles. Currently, there are many types of nanoceramic powders, among which nano-yttrium oxide powder is noteworthy. It attracts attention for its excellent properties, such as good mechanical strength, elastic modulus, heat resistance, catalytic activity, and stability. Nano-yttrium oxide powder has a high melting point, high hardness, and high corrosion resistance, while also possessing high insulation properties and thermal conductivity. It exhibits excellent compatibility with ceramic matrix materials and is considered a promising ceramic powder material.

[0003] Chinese patent "An Industrialized Preparation Method of Nano-Yttrium Oxide for Electronic Ceramics" (Application No.: CN202410734180.X, Publication No.: CN118515305A, Publication Date: 2024-08-20) discloses a method for preparing nano-yttrium oxide for electronic ceramics. This method uses a Y(NO3)3 solution obtained from yttrium oxide and nitric acid solution as the yttrium source, then precipitates yttrium carbonate crystals in two steps using ammonia and ammonium bicarbonate, and finally obtains nano-yttrium oxide through calcination. The nitric acid used in this method is relatively hazardous, and the ammonia solution has a strong odor and involves multiple steps.

[0004] Chinese patent "A Preparation Method of Nano-Yttrium Oxide" (Application No.: CN202410013219.9, Publication No.: CN117819588A, Publication Date: 2024-04-05) discloses a method for preparing nano-yttrium oxide. The method involves using yttrium salt, precipitant, and surfactant to form a solution, then using a multiphase interface reactor and introducing CO2 under stirring to perform carbonation. The precursor slurry is then washed, dispersed in water, and spray-dried. Finally, the obtained nano-yttrium oxide precursor powder is calcined to obtain nano-yttrium oxide powder with small particle size and uniform particle size distribution. However, the process is complex, requires a lot of manual operation, and cannot be automated. Summary of the Invention

[0005] This invention addresses the shortcomings of existing technologies for preparing yttrium oxide powder by proposing a simple, easily controllable method for preparing nano-yttrium oxide powder materials that allows for controlled particle size growth of yttrium oxide at high temperatures.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A method for preparing nano-yttrium oxide based on the double-cage effect specifically includes the following steps:

[0008] Step 1, prepare Y(NO3)3 and YCl3 solutions:

[0009] Weigh Y(NO3)3·6H2O or YCl3·6H2O into a beaker and add deionized water. Stir until completely dissolved to obtain Y(NO3)3 solution or YCl3 solution.

[0010] Step 2, prepare C4H6O6 solution:

[0011] Weigh C4H6O6 into a beaker and add deionized water. Stir until completely dissolved to obtain a C4H6O6 solution.

[0012] Step 3, prepare the syrup solution:

[0013] Measure the syrup into a beaker and add deionized water, then stir thoroughly to obtain a syrup solution.

[0014] Step 4, prepare the precursor solution:

[0015] Add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the Y(NO3)3 solution or YCl3 solution obtained in step 1 in sequence, and continue stirring to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution.

[0016] Step 5: Preparation of precursor powder using water bath method:

[0017] The yttrium oxide precursor solution obtained in step 4 was placed in a water bath for water bath. The white precipitate was centrifuged and washed, and then placed in an oven to dry to obtain yttrium oxide precursor powder.

[0018] Step 6: High-temperature sintering to prepare nano-yttrium oxide materials:

[0019] The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air to obtain nano-yttrium oxide particles.

[0020] Further, in step 1, Y(NO3)3·6H2O or YCl3·6H2O is prepared with deionized water to form a solution of 0.5-1.5 mol / L. The stirring process is carried out using a magnetic stirrer for 10-60 min.

[0021] Furthermore, in step 2, C4H6O6 and deionized water are prepared into a solution of 1-3.5 mol / L, and the stirring process is carried out using a magnetic stirrer for 10-60 min.

[0022] Furthermore, in step 3, the volume ratio of syrup to deionized water is 1:2 to 1:1, and the stirring process is carried out using a magnetic stirrer for 10-60 minutes.

[0023] Furthermore, the characteristic feature is that the stirring process in step 4 is carried out using a magnetic stirrer, and the stirring time is 10-60 minutes.

[0024] Furthermore, in step 5, the water bath conditions are 80℃ for 3-5 hours; during centrifugation and washing, the product is first washed 3 times with ultrapure water, then washed 3 times with anhydrous ethanol; finally, it is dried in a 60℃ oven for 24-48 hours to obtain yttrium oxide precursor powder.

[0025] Furthermore, in step 6, the high-temperature calcination temperature is 700℃-1400℃, and the holding time is 60min.

[0026] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0027] 1. This invention provides a method for preparing nano-yttrium oxide based on the double-cage effect. Yttrium nitrate (Y(NO3)3·6H2O) or yttrium chloride (YCl3·6H2O) is used as the yttrium source. Food-grade additive tartaric acid (C4H6O6) is used as a "cage" as a chelating agent to directly chelate with metal ions, thus encapsulating the metal Y in a cage-like structure. 3+ Using syrup as an adjuvant, a "double cage" is formed on the outside of the chelating agent. The double-cage structure has a lower binding energy than the single-cage structure, ranging from -4.81 × 10⁻⁶. 6 kJ / mol decreased to -9.54 × 10 6 The system is more stable with kJ / mol, which can further stabilize the growth of crystal nuclei. The double cage structure regulates its uniform nucleation and yields the yttrium oxide precursor. This invention uses food-grade tartaric acid and syrup, which are odorless and safe reagents, in line with the national advocacy of green technology innovation.

[0028] 2. During subsequent high-temperature calcination, the double cages can effectively control the growth of nano-yttrium oxide grains. At the same time, the protection of the double cages during high-temperature pyrolysis can improve the ceramic conversion rate.

[0029] 3. The synthesis process of this invention mainly uses inexpensive and readily available inorganic salts and food-grade additives, resulting in low cost, environmentally friendly and safe reagents, a simple and easy-to-implement process with excellent reproducibility, and ease of large-scale industrial production. The method of this invention features a simple and easy-to-implement synthesis process, low synthesis temperature, good reproducibility, and high purity of the synthesized product, making it suitable for applications in functional ceramics and other fields, with broad application prospects. Attached Figure Description

[0030] Figure 1 A flowchart of a method for preparing nano-yttrium oxide based on the double-cage effect provided by the present invention;

[0031] Figure 2 This is a theoretical calculation simulation diagram of the method used in this invention;

[0032] Figure 3 The X-ray diffraction pattern of the nano-yttrium oxide material prepared in Example 3 of this invention;

[0033] Figure 4 Scanning electron microscope images of nano-yttrium oxide materials prepared at different calcination temperatures for samples without added syrup;

[0034] Figure 5 These are scanning electron microscope (SEM) images of nano-yttrium oxide materials prepared at different calcination temperatures in Examples 1-4 of this invention.

[0035] Figure 6 This is a transmission electron microscope (TEM) image of the nano-yttrium oxide material prepared in Example 1 of the present invention. Detailed Implementation

[0036] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] This invention provides a method for preparing nano-yttrium oxide based on the double-cage effect, such as... Figure 1 As shown in the flowchart, the specific operation steps are as follows:

[0038] Step 1, prepare Y(NO3)3 solution or YCl3 solution: Weigh 9.575-28.725g Y(NO3)3·6H2O or 7.582-22.745g YCl3·6H2O into a beaker and add 50mL of deionized water to prepare a 0.5-1.5mol / L solution. Stir with a magnetic stirrer for 10-60min to obtain Y(NO3)3 solution or YCl3 solution.

[0039] Step 2, prepare C4H6O6 solution: Weigh 7.542-26.397g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 1-3.5mol / L solution. Stir with a magnetic stirrer for 10-60min to obtain the C4H6O6 solution.

[0040] Step 3, prepare the syrup solution: Measure the syrup into a beaker and add deionized water. The volume ratio of syrup to deionized water is 1:2-1:1. Stir with a magnetic stirrer for 10-60 minutes to obtain the syrup solution.

[0041] Step 4, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the Y(NO3)3 solution or YCl3 solution obtained in step 1 in sequence, and stir with a magnetic stirrer for 10-60 minutes. The resulting light yellow turbid liquid is the yttrium oxide precursor solution.

[0042] Step 5, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath at 80°C for 3-5 hours. The resulting white precipitate is centrifuged and washed. During centrifugation and washing, the precipitate is first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it is placed in a 60°C oven and dried for 24-48 hours to obtain yttrium oxide precursor powder.

[0043] Step 6, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air. The calcination temperature is 700℃-1400℃ and the holding time is 60min to obtain nano-yttrium oxide particles.

[0044] The method used in this invention is subjected to theoretical calculations and simulations, such as... Figure 2 As shown, C4H6O6 acts as a "cage" chelating agent, directly chelating with metal ions and encapsulating the metal Y in a cage-like structure. 3+ The binding energy at this point is -4.81 × 10⁻⁶. 6 kJ / mol. Using syrup as an adjuvant, a "double cage" is formed on the outside of the chelating agent through grafting; the binding energy at this point is -9.54 × 10⁻⁶ kJ / mol. 6 Based on the thermodynamic principle that the lower the energy, the more stable the structure, the higher the stability of the two-cage structure. This indicates that the two-cage structure regulates the uniform nucleation and yields nano-yttrium oxide precursors.

[0045] Example 1

[0046] Step 1, prepare Y(NO3)3 solution: Weigh 9.575g Y(NO3)3·6H2O into a beaker and add 50mL of deionized water to prepare a 0.5mol / L solution. Stir with a magnetic stirrer for 10min to obtain Y(NO3)3 solution.

[0047] Step 2, prepare C4H6O6 solution: Weigh 7.542g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 1mol / L solution. Stir with a magnetic stirrer for 10min to obtain C4H6O6 solution.

[0048] Step 3, prepare the syrup solution: Measure 20 mL of food-grade additive syrup into a beaker and add 40 mL of deionized water. Stir with a magnetic stirrer for 10 min to obtain the syrup solution.

[0049] Step 4, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the Y(NO3)3 solution obtained in step 1 in sequence, stir with a magnetic stirrer for 10 minutes, and the light yellow turbid liquid obtained is the yttrium oxide precursor solution.

[0050] Step 5, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath at 80°C for 3 hours. The resulting white precipitate is centrifuged and washed. During centrifugation and washing, the precipitate is first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it is placed in a 60°C oven and dried for 24 hours to obtain yttrium oxide precursor powder.

[0051] Step 6, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at 700℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0052] The morphology and structure of the yttrium oxide nanomaterial prepared in Example 1 of this invention were analyzed using transmission electron microscopy (TEM), such as... Figure 6 As shown, Figure 6 (a) Figure 6 (b) Transmission electron microscopy images of yttrium oxide nanoparticles at different locations under the same magnification. Figure 6 (c) are transmission electron microscope images of yttrium oxide nanoparticles at different magnifications. It can be seen that the yttrium oxide nanoparticles calcined at 700℃ have a uniform size distribution, basically around 17 nm. Figure 6 (d) is a high-resolution transmission electron microscope (HRTEM) image, which shows that the interplanar spacing of the nano-yttrium oxide particles calcined at 700℃ is 0.3041 nm, which is consistent with the (222) crystal plane represented by the highest characteristic peak of the yttrium oxide standard card (JCPDS: 41-1105), proving that the method of the present invention can successfully prepare nano-yttrium oxide materials with uniform size.

[0053] Comparative Example 1

[0054] Step 1, prepare Y(NO3)3 solution: Weigh 9.575g Y(NO3)3·6H2O into a beaker and add 50mL of deionized water to prepare a 0.5mol / L solution. Stir with a magnetic stirrer for 10min to obtain Y(NO3)3 solution.

[0055] Step 2, prepare C4H6O6 solution: Weigh 7.542g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 1mol / L solution. Stir with a magnetic stirrer for 10min to obtain C4H6O6 solution.

[0056] Step 3, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 to the Y(NO3)3 solution obtained in step 1, stir with a magnetic stirrer for 10 minutes, and the resulting white turbid liquid is the yttrium oxide precursor solution;

[0057] Step 4, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath at 80°C for 3 hours. The white precipitate is centrifuged and washed. During centrifugation and washing, the precipitate is first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it is placed in a 60°C oven and dried for 24 hours to obtain yttrium oxide precursor powder.

[0058] Step 5, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 4 is placed in a muffle furnace and calcined at high temperature in air at 700℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0059] Example 2

[0060] Step 1, prepare YCl3 solution: Weigh 12.770g YCl3·6H2O into a beaker and add 50mL of deionized water to prepare a 0.8mol / L solution. Stir with a magnetic stirrer for 30min to obtain YCl3 solution;

[0061] Step 2, prepare C4H6O6 solution: Weigh 15.084g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 2mol / L solution. Stir with a magnetic stirrer for 30min to obtain C4H6O6 solution.

[0062] Step 3, prepare the syrup solution: Measure 30 mL of food-grade additive syrup into a beaker and add 40 mL of deionized water. Stir with a magnetic stirrer for 30 min to obtain the syrup solution.

[0063] Step 4, prepare the precursor solution: Add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the YCl3 solution obtained in step 1 in sequence, and stir with a magnetic stirrer for 30 minutes to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution.

[0064] Step 5, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath at 80°C for 4 hours. The resulting white precipitate is centrifuged and washed. During centrifugation and washing, the precipitate is first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it is placed in a 60°C oven and dried for 30 hours to obtain yttrium oxide precursor powder.

[0065] Step 6, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at 800℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0066] Comparative Example 2

[0067] Step 1, prepare YCl3 solution: Weigh 12.770g YCl3·6H2O into a beaker and add 50mL of deionized water to prepare a 0.8mol / L solution. Stir with a magnetic stirrer for 30min to obtain YCl3 solution;

[0068] Step 2, prepare C4H6O6 solution: Weigh 15.084g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 2mol / L solution. Stir with a magnetic stirrer for 30min to obtain C4H6O6 solution.

[0069] Step 3, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 to the YCl3 solution obtained in step 1, and stir with a magnetic stirrer for 30 minutes to obtain a white turbid liquid, which is the yttrium oxide precursor solution;

[0070] Step 4, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 3 was placed in a water bath at 80°C for 4 hours. The resulting white precipitate was centrifuged and washed. During centrifugation and washing, the precipitate was first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it was placed in a 60°C oven and dried for 30 hours to obtain yttrium oxide precursor powder.

[0071] Step 5, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 4 is placed in a muffle furnace and calcined at high temperature in air at 800℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0072] Example 3

[0073] Step 1, prepare Y(NO3)3 solution: Weigh 24.192g Y(NO3)3·6H2O into a beaker and add 50mL of deionized water to prepare a 1.2mol / L solution. Stir with a magnetic stirrer for 10min to obtain Y(NO3)3 solution.

[0074] Step 2, prepare C4H6O6 solution: Weigh 22.626g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 3mol / L solution. Stir with a magnetic stirrer for 10min to obtain C4H6O6 solution.

[0075] Step 3, prepare the syrup solution: Measure 40 mL of food-grade additive syrup into a beaker and add 40 mL of deionized water. Stir with a magnetic stirrer for 10 min to obtain the syrup solution.

[0076] Step 4, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the Y(NO3)3 solution obtained in step 1 in sequence, stir with a magnetic stirrer for 10 minutes, and the light yellow turbid liquid obtained is the yttrium oxide precursor solution.

[0077] Step 5, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath at 80°C for 5 hours. The white precipitate is centrifuged and washed. During centrifugation and washing, the precipitate is first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it is placed in a 60°C oven and dried for 48 hours to obtain yttrium oxide precursor powder.

[0078] Step 6, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at 1200℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0079] X-ray diffraction (XRD) analysis was performed on the nano-yttrium oxide material prepared in Example 3 of this invention, as follows: Figure 3 As shown in the figure, the characteristic peaks of yttrium oxide appear in the nanomaterial and correspond to its standard card (JCPDS: 41-1105). The prepared nano-yttrium oxide material has good crystallinity and is basically free of impurity phases. Therefore, it can be concluded that nano-yttrium oxide material was successfully prepared by the method of this invention.

[0080] Comparative Example 3

[0081] Step 1, prepare Y(NO3)3 solution: Weigh 24.192g Y(NO3)3·6H2O into a beaker and add 50mL of deionized water to prepare a 1.2mol / L solution. Stir with a magnetic stirrer for 10min to obtain Y(NO3)3 solution.

[0082] Step 2, prepare C4H6O6 solution: Weigh 22.626g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 3mol / L solution. Stir with a magnetic stirrer for 10min to obtain C4H6O6 solution.

[0083] Step 3, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 to the Y(NO3)3 solution obtained in step 1, stir with a magnetic stirrer for 10 minutes, and the resulting white turbid liquid is the yttrium oxide precursor solution;

[0084] Step 4, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 3 was placed in a water bath at 80°C for 5 hours. The white precipitate was centrifuged and washed. During centrifugation and washing, the precipitate was first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it was placed in a 60°C oven and dried for 48 hours to obtain yttrium oxide precursor powder.

[0085] Step 5, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 4 is placed in a muffle furnace and calcined at high temperature in air at 1200℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0086] Example 4

[0087] Step 1, prepare YCl3 solution: Weigh 22.745g YCl3·6H2O into a beaker and add 50mL of deionized water to prepare a 1.5mol / L solution. Stir with a magnetic stirrer for 60min to obtain YCl3 solution.

[0088] Step 2, prepare C4H6O6 solution: Weigh 26.397g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 3.5mol / L solution. Stir with a magnetic stirrer for 60min to obtain C4H6O6 solution.

[0089] Step 3, prepare the syrup solution: Measure 40 mL of food-grade additive syrup into a beaker and add 40 mL of deionized water. Stir with a magnetic stirrer for 60 min to obtain the syrup solution.

[0090] Step 4, prepare the precursor solution: Add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the YCl3 solution obtained in step 1 in sequence, and stir with a magnetic stirrer for 60 minutes to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution.

[0091] Step 5, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath at 80°C for 4 hours. The resulting white precipitate is centrifuged and washed. During centrifugation and washing, the precipitate is first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it is placed in a 60°C oven and dried for 30 hours to obtain yttrium oxide precursor powder.

[0092] Step 6, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at 1400℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0093] Comparative Example 4

[0094] Step 1, prepare YCl3 solution: Weigh 22.745g YCl3·6H2O into a beaker and add 50mL of deionized water to prepare a 1.5mol / L solution. Stir with a magnetic stirrer for 60min to obtain YCl3 solution.

[0095] Step 2, prepare C4H6O6 solution: Weigh 26.397g of C4H6O6 into a beaker and add 50mL of deionized water to prepare a 3.5mol / L solution. Stir with a magnetic stirrer for 60min to obtain C4H6O6 solution.

[0096] Step 3, prepare the precursor solution: add the C4H6O6 solution obtained in step 2 to the YCl3 solution obtained in step 1, and stir with a magnetic stirrer for 60 minutes to obtain a white turbid liquid, which is the yttrium oxide precursor solution;

[0097] Step 4, Preparation of precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 3 was placed in a water bath at 80°C for 4 hours. The resulting white precipitate was centrifuged and washed. During centrifugation and washing, the precipitate was first washed 3 times with ultrapure water and then washed 3 times with anhydrous ethanol. Finally, it was placed in a 60°C oven and dried for 30 hours to obtain yttrium oxide precursor powder.

[0098] Step 5, high-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 4 is placed in a muffle furnace and calcined at high temperature in air at 1400℃ for 60 minutes to obtain nano-yttrium oxide particles.

[0099] The morphology of the yttrium oxide nanomaterials prepared in Examples 1-4 of this invention was analyzed using scanning electron microscopy (SEM) compared with that of the yttrium oxide nanomaterials prepared in Comparative Examples 1-4 without the addition of syrup as a reaction aid. Figure 4 and 5 As shown, Figure 4 (a) Scanning electron microscope image of yttrium oxide nanomaterials prepared without syrup at a calcination temperature of 700℃. Figure 4 (b) Scanning electron microscope image of yttrium oxide nanomaterials prepared without sugar at a calcination temperature of 800℃. Figure 4 (c) Scanning electron microscope image of yttrium oxide nanomaterials prepared without syrup at a calcination temperature of 1200℃. Figure 4(d) is a scanning electron microscope image of nano-yttrium oxide material prepared without syrup at a calcination temperature of 1400℃. Figure 5 (a) is a scanning electron microscope image of nano-yttrium oxide material prepared in Example 1 at a calcination temperature of 700℃. Figure 5 (b) Scanning electron microscope image of nano-yttrium oxide material prepared in Example 2 at a calcination temperature of 800℃. Figure 5 (c) is a scanning electron microscope image of the nano-yttrium oxide material prepared in Example 3 at a calcination temperature of 1200℃. Figure 5 (d) is a scanning electron microscope image of nano-yttrium oxide material prepared in Example 4 at a calcination temperature of 1400℃.

[0100] from Figure 4 and 5 It can be seen that the nano-yttrium oxide particles prepared by adding syrup as a reaction aid are uniformly distributed. As the calcination temperature increases, the grains gradually grow. Compared with the nano-yttrium oxide particles prepared without adding syrup as a reaction aid, the grain growth is controlled, proving that the method of the present invention can successfully prepare nano-yttrium oxide materials with controlled grain growth at high temperature.

[0101] The conversion rate of nano-yttrium oxide powder was obtained by measuring the mass loss before and after calcination at different temperatures, as shown in Table 1. It can be seen that using C4H6O6 as "one cage" and syrup as "two cages" can also reduce the loss rate of precursors during calcination.

[0102] Table 1

[0103]

[0104] The grain size of nano-yttrium oxide powder obtained by calcination at different temperatures was calculated using the Scherrer formula, as shown in Table 2. It can be seen that using C4H6O6 as "one cage" and syrup as "two cages" can control the grain growth that occurs with the increase of calcination temperature.

[0105] Table 2

[0106]

[0107] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing nano-yttrium oxide based on the double-cage effect, characterized in that, Specifically, the following steps are included: Step 1, prepare Y(NO3)3 and YCl3 solutions: Weigh Y(NO3)3·6H2O or YCl3·6H2O into a beaker and add deionized water. Stir until completely dissolved to obtain Y(NO3)3 solution or YCl3 solution. Step 2, prepare C4H6O6 solution: Weigh C4H6O6 into a beaker and add deionized water. Stir until completely dissolved to obtain a C4H6O6 solution. Step 3, prepare the syrup solution: Measure the syrup into a beaker and add deionized water, then stir thoroughly to obtain a syrup solution. Step 4, prepare the precursor solution: Add the C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 to the Y(NO3)3 solution or YCl3 solution obtained in step 1 in sequence, and continue stirring to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution. Step 5: Preparation of precursor powder using water bath method: The yttrium oxide precursor solution obtained in step 4 was placed in a water bath for water bath. The white precipitate was centrifuged and washed, and then placed in an oven to dry to obtain yttrium oxide precursor powder. Step 6: High-temperature sintering to prepare nano-yttrium oxide materials: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air to obtain nano-yttrium oxide particles.

2. The method for preparing nano-yttrium oxide based on the double-cage effect according to claim 1, characterized in that, In step 1, Y(NO3)3·6H2O or YCl3·6H2O is mixed with deionized water to prepare a solution of 0.5-1.5 mol / L. The stirring process is carried out using a magnetic stirrer for 10-60 min.

3. The method for preparing nano-yttrium oxide based on the double-cage effect according to claim 1, characterized in that, In step 2, C4H6O6 and deionized water are mixed to prepare a solution of 1-3.5 mol / L. The stirring process is carried out using a magnetic stirrer for 10-60 min.

4. The method for preparing nano-yttrium oxide based on the double-cage effect according to claim 1, characterized in that, In step 3, the volume ratio of syrup to deionized water is 1:2 to 1:

1. The stirring process is carried out using a magnetic stirrer, and the stirring time is 10-60 minutes.

5. The method for preparing nano-yttrium oxide based on the double-cage effect according to claim 1, characterized in that, In step 4, the mixing process is carried out using a magnetic stirrer, and the mixing time is 10-60 minutes.

6. The method for preparing nano-yttrium oxide based on the double-cage effect according to claim 1, characterized in that, In step 5, the water bath conditions are 80 ℃ for 3-5 h; during centrifugation and washing, the product is first washed 3 times with ultrapure water, then washed 3 times with anhydrous ethanol; finally, it is dried in a 60 ℃ oven for 24-48 h to obtain yttrium oxide precursor powder.

7. The method for preparing nano-yttrium oxide based on the double-cage effect according to claim 1, characterized in that, In step 6, the high-temperature calcination temperature is 700 ℃-1400 ℃, and the holding time is 60 min.

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