Method for preparing nano yttrium oxide based on double-cage effect

Abstract

According to the method, Y (NO3) 3.6 H2O or YCl3. 6H2O is taken as yttrium salt, C4H6O6 is taken as a'one-cage 'reaction chelating agent to be directly chelated with metal ions, metal Y < 3 + > is coated with a cage-shaped structure, syrup is taken as an auxiliary agent to be grafted outside the chelating agent to form a'two-cage', crystal nucleus growth is stabilized, and the nano yttrium oxide is prepared. The uniform nucleation of yttrium oxide is regulated and controlled by a double-cage structure, and the growth speed of crystals is controlled through a water bath reaction under a high-concentration acidic condition, so that a nano yttrium oxide material is successfully prepared; in the synthesis process, inorganic salt and food-grade additives which are low in cost and easy to obtain are used as raw materials, the cost is low, reagents are environment-friendly and safe, the green technology innovation advocated by the double-carbon strategy is met, the method is simple and easy to implement, the repeatability is good, large-scale production can be achieved, and the commercialization process of functional ceramic materials can be effectively promoted.

Description

Technical Field

[0001] The invention belongs to the technical field of ceramic materials, and in particular relates to a method for preparing nano yttrium oxide based on a double cage effect. Background Art

[0002] Nano ceramic powder is a substance with nanometer size between solid and molecule. Nano powder material has extremely small particle size, large specific surface area and high chemical properties, which can significantly reduce the sintering temperature of materials and save energy. Nano-scale powder is conducive to improving the density of ceramic materials and improving the mechanical properties of ceramic materials. At the same time, due to its small powder particle size, if the grains grow evenly during the firing process, some unique properties that large particle materials do not have may appear. At present, there are many types of nano ceramic powders, and nano yttrium oxide powder is one of them. It attracts attention for its excellent properties, such as good mechanical strength, elastic modulus, heat resistance, catalysis and stability. Nano yttrium oxide powder has high melting point, high hardness and high corrosion resistance, as well as high insulation performance and thermal conductivity. It has good compatibility with ceramic matrix materials and is considered to be a very promising ceramic powder material.

[0003] The Chinese patent "An Industrial Preparation Method of Nano-yttrium Oxide for Electronic Ceramics" (application number: CN202410734180.X, authorization number: CN118515305A, announcement date: 2024-08-20) discloses a method for preparing nano-yttrium oxide for electronic ceramics. The method uses yttrium oxide and nitric acid solution to obtain Y(NO3)3 solution as the yttrium source, and then precipitates yttrium carbonate crystals in two steps through ammonia water and ammonium bicarbonate, and calcines to obtain nano-yttrium oxide. The nitric acid used in this method is relatively dangerous, the ammonia water has a strong odor, and there are many steps.

[0004] The Chinese patent "A method for preparing nano yttrium oxide" (application number: CN202410013219.9, authorization number: CN117819588A, announcement date: 2024-04-05) discloses a method for preparing nano yttrium oxide. The method uses yttrium salt, precipitant and surfactant to compound into a solution, and then uses a multiphase interface reactor, and introduces CO2 under stirring for carbonation, and then washes the precursor slurry and disperses it with water for spray drying. 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, but its process is complicated, requires a lot of manual operation, and cannot be produced automatically. Summary of the invention

[0005] Aiming at the shortcomings of the prior art in preparing yttrium oxide powder, the present invention provides a method for preparing a nano yttrium oxide powder material with simple steps, easy-to-control process and the ability to control the growth of yttrium oxide particles at high temperature.

[0006] To achieve the above object, the present invention adopts the following technical solutions:

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

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

[0009] Weigh Y(NO3)3·6H2O or YCl3·6H2O into a beaker and add deionized water, stirring 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, stirring until completely dissolved to obtain a C4H6O6 solution;

[0012] Step 3, prepare 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] The C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 are sequentially added to the Y(NO3)3 solution or YCl3 solution obtained in step 1, and the light yellow turbid solution obtained by continuous stirring is the yttrium oxide precursor solution;

[0016] Step 5, preparing precursor powder by water bath method:

[0017] The yttrium oxide precursor solution obtained in step 4 is placed in a water bath, the obtained white precipitate is centrifugally washed and then placed in an oven for drying to obtain yttrium oxide precursor powder;

[0018] Step 6, high temperature sintering to prepare nano yttrium oxide material:

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

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

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

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

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

[0024] Furthermore, the water bath condition in step 5 is 80° C. for 3-5 hours; during centrifugal washing, first wash with ultrapure water for 3 times, and then wash with anhydrous ethanol for 3 times; finally, place in a 60° C. oven and dry for 24-48 hours to obtain yttrium oxide precursor powder.

[0025] Furthermore, in step 6, the high temperature calcination temperature is 700° C.-1400° C., and the insulation time is 60 minutes.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] 1. The present invention provides a method for preparing nano yttrium oxide based on the double cage effect, using yttrium nitrate (Y(NO3)3·6H2O) or yttrium chloride (YCl3·6H2O) as the yttrium source, using food grade additive tartaric acid (C4H6O6) as a "cage" as a reaction chelating agent to directly chelate with metal ions, and coating metal Y with a cage structure. 3+ The syrup was used as an auxiliary agent to graft onto the outside of the chelating agent to form a "double cage". The double cage structure has lower binding energy than the single cage structure, from -4.81×10 6 kJ / mol decreased to -9.54×10 6 kJ / mol, the system is more stable, the growth of the crystal nucleus can be further stabilized, and the double cage structure regulates its uniform nucleation to obtain an yttrium oxide precursor. The present invention uses food-grade tartaric acid and syrup, which are odorless and reagents are safe, and is in line with the green technology innovation concept advocated by the country.

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

[0029] 3. The synthesis process of the present invention mainly uses inexpensive and readily available inorganic salts and food-grade additives, which is low in cost, environmentally friendly and safe, and the process is simple and easy to operate with good repeatability, which is easy to achieve large-scale industrial production. The method of the present invention has a simple and easy synthesis process, low synthesis temperature, good repeatability, and high purity of the synthesized product, which can be used in functional ceramics and other aspects, and has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 A flow chart 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 the present invention;

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

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

[0034] Figure 5 The scanning electron microscope images of the nano-yttrium oxide materials prepared in Examples 1-4 of the present invention at different calcination temperatures;

[0035] Figure 6 This is a transmission electron microscope image of the nano yttrium oxide material prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0036] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] The present invention provides a method for preparing nano yttrium oxide based on the double cage effect, such as Figure 1 As shown in the flow chart, the specific 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 in a beaker and add 50mL deionized water to prepare a 0.5-1.5mol / L solution, stir with a magnetic stirrer for 10-60min to obtain a Y(NO3)3 solution or a YCl3 solution;

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

[0040] Step 3, preparing a syrup solution: measuring the syrup into a beaker, adding deionized water, the volume ratio of the syrup to the deionized water being 1:2-1:1, and stirring with a magnetic stirrer for 10-60 minutes to obtain a syrup solution;

[0041] Step 4, preparing a precursor solution: adding 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, stirring for 10-60 minutes using a magnetic stirrer, and the obtained light yellow turbid solution is the yttrium oxide precursor solution;

[0042] Step 5, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 4 in a water bath at 80°C for 3-5h, centrifuging and washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in a 60°C oven for 24-48h to obtain yttrium oxide precursor powder;

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

[0044] The method used in the present invention is simulated by theoretical calculation, such as Figure 2 As shown in the figure, it can be seen that C4H6O6 is a "cage" as a reaction chelating agent to directly chelate with metal ions, encapsulating metal Y with a cage structure 3+ , the binding energy at this time is -4.81×10 6 kJ / mol. Using syrup as an auxiliary agent to graft onto the outside of the chelating agent to form a "second cage", the binding energy at this time is -9.54×10 6 kJ / mol. According to the thermodynamic principle that the lower the energy, the more stable the structure, it is confirmed that the two-cage structure is more stable than the one-cage structure, indicating that the double-cage structure regulates its uniform nucleation and obtains a nano-yttrium oxide precursor.

[0045] Example 1

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

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

[0048] Step 3, preparing a syrup solution: measuring 20 mL of food-grade additive syrup into a beaker and adding 40 mL of deionized water, stirring with a magnetic stirrer for 10 minutes to obtain a syrup solution;

[0049] Step 4, preparing a precursor solution: adding 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, stirring for 10 minutes using a magnetic stirrer to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution;

[0050] Step 5, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 4 in a water bath at 80°C for 3 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 24 hours to obtain yttrium oxide precursor powder;

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

[0052] The morphology and structure of the nano-yttrium oxide material prepared in Example 1 of the present invention were analyzed using a transmission electron microscope (TEM). Figure 6 As shown, Figure 6 (a) Figure 6 (b) is a transmission electron microscope photo of nano-yttrium oxide particles at different positions at the same magnification. Figure 6 (c) is a transmission electron microscope photo of nano-yttrium oxide particles at different magnifications. It can be seen that the size of the nano-yttrium oxide particles calcined at 700°C is uniformly distributed, basically around 17nm. Figure 6 (d) is a high-resolution transmission electron microscope (HRTEM) photograph, from which it can be seen that the interplanar spacing of the nano-yttrium oxide particles calcined at 700°C 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 deionized water to prepare a 0.5mol / L solution, stir with a magnetic stirrer for 10min to obtain a Y(NO3)3 solution;

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

[0056] Step 3, preparing a precursor solution: adding the C4H6O6 solution obtained in step 2 to the Y(NO3)3 solution obtained in step 1, stirring for 10 minutes using a magnetic stirrer to obtain a white turbid solution, which is the yttrium oxide precursor solution;

[0057] Step 4, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 4 in a water bath at 80°C for 3 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in a 60°C oven for 24 hours to obtain yttrium oxide precursor powder;

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

[0059] Example 2

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

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

[0062] Step 3, preparing a syrup solution: measuring 30 mL of food-grade additive syrup into a beaker and adding 40 mL of deionized water, stirring with a magnetic stirrer for 30 minutes to obtain a syrup solution;

[0063] Step 4, preparing a precursor solution: adding 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, stirring with a magnetic stirrer for 30 minutes to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution;

[0064] Step 5, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 4 in a water bath at 80°C for 4 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 30 hours to obtain yttrium oxide precursor powder;

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

[0066] Comparative Example 2

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

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

[0069] Step 3, preparing a precursor solution: adding the C4H6O6 solution obtained in step 2 to the YCl3 solution obtained in step 1, stirring for 30 minutes using a magnetic stirrer to obtain a white turbid liquid, which is the yttrium oxide precursor solution;

[0070] Step 4, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 3 in a water bath at 80°C for 4 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 30 hours to obtain yttrium oxide precursor powder;

[0071] Step 5, high-temperature sintering to prepare nano-yttrium oxide material: the yttrium oxide precursor powder obtained in step 4 is placed in a muffle furnace and calcined at high temperature in air at a calcination temperature of 800° C. 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 deionized water to prepare a 1.2mol / L solution, stir with a magnetic stirrer for 10min to obtain a Y(NO3)3 solution;

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

[0075] Step 3, preparing a syrup solution: measuring 40 mL of food-grade additive syrup into a beaker and adding 40 mL of deionized water, stirring with a magnetic stirrer for 10 minutes to obtain a syrup solution;

[0076] Step 4, preparing a precursor solution: adding 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, stirring for 10 minutes using a magnetic stirrer to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution;

[0077] Step 5, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 4 in a water bath at 80°C for 5 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 48 hours to obtain yttrium oxide precursor powder;

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

[0079] X-ray diffraction analysis (XRD) was performed on the nano yttrium oxide material prepared in Example 3 of the present invention. Figure 3 As shown in the figure, it can be seen that the characteristic peaks of yttrium oxide appear in the nano material and correspond to its standard card (JCPDS: 41-1105). The prepared nano yttrium oxide material has good crystallinity and basically no impurity phase. Therefore, it can be concluded that the nano yttrium oxide material is successfully prepared by the method of the present 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 deionized water to prepare a 1.2mol / L solution, stir with a magnetic stirrer for 10min to obtain a Y(NO3)3 solution;

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

[0083] Step 3, preparing a precursor solution: adding the C4H6O6 solution obtained in step 2 to the Y(NO3)3 solution obtained in step 1, stirring for 10 minutes using a magnetic stirrer to obtain a white turbid solution, which is the yttrium oxide precursor solution;

[0084] Step 4, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 3 in a water bath at 80°C for 5 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 48 hours to obtain yttrium oxide precursor powder;

[0085] Step 5, high-temperature sintering to prepare nano-yttrium oxide material: the yttrium oxide precursor powder obtained in step 4 is placed in a muffle furnace and calcined at high temperature in air at a calcination temperature of 1200° C. 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 deionized water to prepare a 1.5mol / L solution, stir with a magnetic stirrer for 60min to obtain a YCl3 solution;

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

[0089] Step 3, preparing a syrup solution: measuring 40 mL of food-grade additive syrup into a beaker and adding 40 mL of deionized water, stirring with a magnetic stirrer for 60 minutes to obtain a syrup solution;

[0090] Step 4, preparing a precursor solution: adding 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, stirring for 60 minutes using a magnetic stirrer to obtain a light yellow turbid liquid, which is the yttrium oxide precursor solution;

[0091] Step 5, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 4 in a water bath at 80°C for 4 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 30 hours to obtain yttrium oxide precursor powder;

[0092] Step 6, high-temperature sintering to prepare nano-yttrium oxide material: the yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature in air at a calcination temperature of 1400° C. 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 deionized water to prepare a 1.5mol / L solution, stir with a magnetic stirrer for 60min to obtain a YCl3 solution;

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

[0096] Step 3, preparing a precursor solution: adding the C4H6O6 solution obtained in step 2 to the YCl3 solution obtained in step 1, stirring for 60 minutes using a magnetic stirrer to obtain a white turbid liquid, which is the yttrium oxide precursor solution;

[0097] Step 4, preparing precursor powder by water bath method: placing the yttrium oxide precursor solution obtained in step 3 in a water bath at 80°C for 4 hours, centrifugally washing the obtained white precipitate, first washing it with ultrapure water for 3 times, and then washing it with anhydrous ethanol for 3 times; finally, drying it in an oven at 60°C for 30 hours to obtain yttrium oxide precursor powder;

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

[0099] The morphology of the nano-yttrium oxide materials prepared in Examples 1-4 of the present invention and the nano-yttrium oxide materials prepared in Comparative Examples 1-4 without adding syrup as a reaction aid were analyzed using a scanning electron microscope (SEM). Figure 4 and 5 As shown, Figure 4 (a) is a scanning electron microscope image of nano-yttrium oxide material prepared at a calcination temperature of 700°C without adding syrup. Figure 4 (b) is a scanning electron microscope image of nano-yttrium oxide material prepared at a calcination temperature of 800°C without adding sugar. Figure 4 (c) is a scanning electron microscope image of nano-yttrium oxide material prepared at a calcination temperature of 1200°C without adding syrup. Figure 4(d) is a scanning electron microscope image of nano yttrium oxide material prepared at a calcination temperature of 1400°C without adding syrup. Figure 5 (a) is a scanning electron microscope image of the nano yttrium oxide material prepared at a calcination temperature of 700°C in Example 1. Figure 5 (b) SEM image of nano-yttrium oxide material prepared at 800°C in Example 2. Figure 5 (c) is a scanning electron microscope image of the nano yttrium oxide material prepared at a calcination temperature of 1200°C in Example 3. Figure 5 (d) is a scanning electron microscope image of the nano yttrium oxide material prepared at a calcination temperature of 1400°C in Example 4.

[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 evenly distributed, and 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 temperatures.

[0101] The conversion rate of nano yttrium oxide powder was obtained by 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 the precursor during the calcination process.

[0102] Table 1

[0103]

[0104] The grain size of nano yttrium oxide powder calcined at different temperatures was calculated by Scherrer's 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 present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing nano yttrium oxide based on double cage effect, characterized in that: The specific steps include: Step 1, prepare Y(NO3)3, YCl3 solution: Weigh Y(NO3)3·6H2O or YCl3·6H2O into a beaker and add deionized water, stirring 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, stirring until completely dissolved to obtain a C4H6O6 solution; Step 3, prepare syrup solution: Measure the syrup into a beaker and add deionized water, stir thoroughly to obtain a syrup solution; Step 4, prepare the precursor solution: The C4H6O6 solution obtained in step 2 and the syrup solution obtained in step 3 are sequentially added to the Y(NO3)3 solution or YCl3 solution obtained in step 1, and the light yellow turbid solution obtained by continuous stirring is the yttrium oxide precursor solution; Step 5, preparing precursor powder by water bath method: The yttrium oxide precursor solution obtained in step 4 is placed in a water bath, the obtained white precipitate is centrifugally washed and then placed in an oven for drying to obtain yttrium oxide precursor powder; Step 6, high temperature sintering to prepare nano yttrium oxide material: The yttrium oxide precursor powder obtained in step 5 is placed in a muffle furnace and calcined at high temperature under 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 and deionized water are prepared into a 0.5-1.5 mol / L solution, and the stirring process is carried out using a magnetic stirrer for a stirring time of 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 configured into a 1-3.5 mol / L solution, and the stirring process is carried out using a magnetic stirrer for a stirring time of 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 1:2-1:1, and the stirring process is carried out using a magnetic stirrer for 10-60 minutes.

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

6. The method for preparing nano yttrium oxide ceramic particles according to claim 1, characterized in that: The water bath condition in step 5 is 80° C. for 3-5 hours; during centrifugal washing, first wash with ultrapure water for 3 times, and then wash with anhydrous ethanol for 3 times; finally, place in a 60° C. oven and dry for 24-48 hours to obtain yttrium oxide precursor powder.

7. The method for preparing nano yttrium oxide ceramic particles according to claim 1, characterized in that: In step 6, the high temperature calcination temperature is 700° C.-1400° C., and the insulation time is 60 minutes.

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