CN111977688B - Controllable NaVO preparation 2 Method for preparing nanosphere sodium storage electrode material - Google Patents
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Abstract
The invention relates to the field of nanotechnology, and discloses a controllable preparation method of NaVO 2 A method for preparing a nanosphere sodium storage electrode material. The method takes sodium salt and vanadium pentoxide as raw materials, and prepares NaVO with high purity, uniform size and regular morphology by a method combining high-temperature sintering and microwave radiation 2 Nanosphere material. NaVO (NaVO) 2 The specific area is increased after nano crystallization, so that the sodium storage capacity of the material can be effectively improved, and the material performance is optimized. The invention simplifies the preparation steps, shortens the reaction time, reduces the preparation cost and provides a new idea for synthesizing the electrode material of the sodium ion battery by adding the microwave radiation method.
Description
Technical Field
The invention relates to the field of nano material preparation, in particular to a controllable preparation method of NaVO 2 A method for preparing a nanosphere sodium storage electrode material.
Technical Field
Sodium ion batteries have been attracting attention in new energy applications due to price advantages, and are considered as one of the ideal choices for the next generation of large-scale energy storage technologies, and development and preparation of battery materials are extremely important. Positive electrode material as an important component of sodium ion batteryDirectly affects the performance and cost of the battery. The positive electrode material of the sodium ion battery is a sodium-embedded compound, such as layered oxide, polyanion oxide, metal framework structure material and the like. NaMO due to layered metal transition oxides 2 (M is a transition metal Mn, V, ni, etc.) has been receiving great attention as a research hotspot for current sodium ion battery materials (T.Wu, J.G.Sun, Z.Q.Jeremy.Yap, M.L.Ke, christina Y.H.Lim, L.Lu, J.Mater.Design.2020, 10, 1016) with excellent electrochemical properties.
NaVO 2 The metal transition oxide has excellent electrochemical performance and high stability due to reversible ion deintercalation capability and stable octahedral crystal structure, and has good development prospect in the field of sodium ion electrode materials. With bulk NaVO 2 In contrast, naVO 2 The properties of the nanostructures, due to quantum effects and small dimensions, allow further optimization of material properties (O.Szajwaj, E.Gaudin, F.Weill, J.Darriet, C.Delmas.J.Inorg.Chem.2009, 48, 9147-9154). NaVO at present 2 Few reports on the aspect of nano material preparation are provided, and the synthesis method of the material mainly comprises a hydrothermal/solvothermal method, a carbothermal reduction method, a hydrogen reduction method and the like (B.P.Yang, C.L.Hu, X.Xu, C.F.Sun, J.H.Zhang, J.G Mao.J. chem. Mater.2010, 22, 1545-1550;Y.J.Chen,Y.L.Xu,X.F.Sun,B.F.Zhang,S.N.He,C.Wang.J.J.Power Sources.2018, 397, 307-317; C.Dier, M.Guignard, C.Denage, O.Szajwai, S.Ito, I.Saadone, J.Darriet, C.Delma.J.electric chem. Solid-State Lett,2011, 14, 75-78). However, the traditional preparation method has the disadvantages of complex operation, high preparation cost and long reaction time. If a preparation method which is easy to operate, low in cost and high in yield can be developed on the basis of the existing research, the NaVO with good shape controllability is obtained 2 NaVO (NaVO) is obviously promoted by the Naball sodium storage electrode material 2 And (3) a large-scale production process of the nanosphere sodium storage electrode material.
It is noted that the microwave radiation method is one of the new preparation methods for synthesizing nano materials in recent years. The traditional high-temperature heating mode utilizes the heat conduction effect, so that the energy loss is high, the efficiency is low, the heating is uneven, the internal temperature of a research target is low, and the reaction is insufficient. Microwave radiation is an internal heat source, and a research target absorbs microwaves to heat the target, so that the microwave is heated uniformly, and the heating reaction time is reduced; the microwave can make atoms and molecules vibrate at high speed, so that more favorable thermodynamic conditions are created for the reaction, and the process energy consumption is reduced; the microwave heating inertia is small, the rapid control of temperature rise and fall can be realized, and the continuous synthesis is facilitated.
Based on the above considerations, the present patent introduces microwave radiation into NaVO 2 In the synthesis system of the nano material, controllable NaVO preparation is carried out by a two-step method of high-temperature sintering and microwave radiation 2 The nanosphere sodium storage electrode material aims to prepare the nano material with high purity, uniform size and regular morphology, and provides a solid theoretical basis and practical experience for efficient synthesis and general application of the material.
Disclosure of Invention
Based on the technical background, the invention provides a controllable preparation method for NaVO 2 A method for preparing a nanosphere sodium storage electrode material. NaVO with regular morphology and uniform size can be prepared by controlling the reaction parameter conditions 2 Nanosphere sodium storage electrode material. In the experiment, the two methods of high-temperature sintering and microwave radiation are combined, so that the operation process is simplified, the preparation cost is reduced, the purity of the product is improved, the repeatability of the reaction is improved, and the NaVO is realized 2 The mass production of the nanosphere sodium storage electrode material has great significance.
In order to achieve the above purpose, the present invention uses the following technical scheme:
first, accurately weigh 10.0000g analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh;
secondly, fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 40-50 ℃, controlling the interval time between forward rotation and reverse rotation of the ball mill to be 15 min, and separating the ball grinding tank and uniform powder materials for 2 h;
thirdly, controlling the vertical pressure to be 10-15 MPa for 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining a precursor compact sheet with the thickness of 4-5 mm and the diameter of 10 mm;
fourthly, placing the precursor compacting sheet obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heat treatment heating order is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color and luster;
fifthly, grinding 0.5000g of the pure phase material into powder to 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to be 200-1500 watts, and heating the system for 4 hours at the reaction temperature of 100 ℃;
sixthly, cooling the suspension to be synthesized to normal temperature, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 3-5 times, and drying to obtain high-purity NaVO 2 Electrode material of nanoparticles.
The NaVO 2 The nano particles are spherical in shape and have the particle size of 50-200 nm.
The NaVO 2 The nanosphere sodium storage electrode material is used as an electrode material of a sodium ion battery.
Advantages and effects of the invention
The invention has the following advantages and beneficial effects: 1. NaVO prepared by adopting method of combining high-temperature sintering and microwave radiation 2 The nanosphere sodium storage electrode material has uniform size, regular morphology and high purity; the synthesized material is nano-scale, large in specific area and high in reactivity, so that the material is a good sodium ion battery anode material. 2. After the reaction is finished, high-temperature calcination is not needed, and the protection of the crystal morphology of the product is facilitated. 3. NaVO prepared by the invention 2 The nanosphere sodium storage electrode material can improve the capacity value of the battery, and the cycle stability of the battery is enhanced, so that the nanosphere sodium storage electrode material has development prospect and development potential. 4. The invention adoptsThe synthesis method has the advantages of simple process, strong product structure controllability, good reaction reproducibility, low preparation cost and the like, and provides a new idea for the synthesis of the nano electrode material.
Drawings
FIG. 1 is NaVO 2 Crystal structure
Detailed Description
Example 1: precursor compact sheet with thickness of 4mm is prepared into NaVO by using 200W microwave radiation power 2 Nanosphere electrode material
Accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 50 ℃, enabling the interval time between the forward rotation and the reverse rotation of the ball mill to be 15 min, enabling the total ball milling time to be 2h, and separating the ball grinding tank and uniform powder materials; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 4mm and the diameter of 10 mm.
Placing the precursor compact obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heating order of heat treatment is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color.
Grinding 0.5000g of the pure phase material into powder of 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to be 200 watts, reacting at 100 ℃ for 4 hours, cooling the suspension to be synthesized, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 5 times, and drying to obtain high-purity NaVO 2 Nanoparticle electrode material 1.
Example 2: precursor compact sheet with thickness of 4mm is prepared into NaVO by using 850W microwave radiation power 2 Nanosphere electrode material
Accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 40 ℃, enabling the interval time between the forward rotation and the reverse rotation of the ball mill to be 15 min, enabling the total ball milling time to be 2h, and separating the ball grinding tank and uniform powder materials; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 4mm and the diameter of 10 mm.
Placing the precursor compact obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heating order of heat treatment is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color.
Grinding 0.5000g of the pure phase material into powder of 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to 850 watts, reacting at 100 ℃ for 4 hours, cooling the suspension to be synthesized, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 5 times, and drying to obtain high-purity NaVO 2 The electrode material 2 of the nanoparticle.
Example 3: precursor compact with thickness of 4mm is prepared into NaVO by using 1500W microwave radiation power 2 Nanosphere electrode material
Accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 50 ℃, enabling the interval time between the forward rotation and the reverse rotation of the ball mill to be 15 min, enabling the total ball milling time to be 2h, and separating the ball grinding tank and uniform powder materials; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 4mm and the diameter of 10 mm.
Placing the precursor compact obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heating order of heat treatment is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color.
Grinding 0.5000g of the pure phase material into powder of 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to be 1500 watts, reacting at 100 ℃ for 4 hours, cooling the suspension to be synthesized, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 5 times, and drying to obtain high-purity NaVO 2 The electrode material 3 of the nanoparticle.
Example 4: precursor compact with thickness of 5mm is prepared into NaVO by using 200W microwave radiation power 2 Nanosphere electrode material
Accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 40 ℃, and controlling the interval time between the forward rotation and the reverse rotation of the ball mill to be 15The total ball milling time is 2 hours, and the ball milling tank and the uniform powder material are separated; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 5mm and the diameter of 10 mm.
Placing the precursor compact obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heating order of heat treatment is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color.
Grinding 0.5000g of the pure phase material into powder of 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to be 200 watts, reacting at 100 ℃ for 4 hours, cooling the suspension to be synthesized, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 5 times, and drying to obtain high-purity NaVO 2 The electrode material 4 of the nanoparticle.
Example 5: precursor compact with thickness of 5mm is prepared into NaVO by using 850W microwave radiation power 2 Nanosphere electrode material
Accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 50 ℃, enabling the interval time between the forward rotation and the reverse rotation of the ball mill to be 15 min, enabling the total ball milling time to be 2h, and separating the ball grinding tank and uniform powder materials; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 5mm and the diameter of 10 mm.
Placing the precursor compact obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heating order of heat treatment is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color.
Grinding 0.5000g of the pure phase material into powder of 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to 850 watts, reacting at 100 ℃ for 4 hours, cooling the suspension to be synthesized, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 5 times, and drying to obtain high-purity NaVO 2 The electrode material 5 of the nanoparticle.
Example 6: precursor compact with thickness of 5mm is prepared into NaVO by using 1500W microwave radiation power 2 Nanosphere electrode material
Accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 50 ℃, enabling the interval time between the forward rotation and the reverse rotation of the ball mill to be 15 min, enabling the total ball milling time to be 2h, and separating the ball grinding tank and uniform powder materials; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 5mm and the diameter of 10 mm.
Placing the precursor compact obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heating order of heat treatment is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color.
Grinding 0.5000g of the pure phase material into 200 mesh powder in a mortar, adding the powder to normal pressure and carrying out beltAdding 50.0ml of distilled water into a 150 ml quartz round-bottom flask of a microwave reactor of a reflux cooling device, controlling the radiation power to be 1500 watts, the reaction temperature to be 100 ℃, heating the system for 4 hours, cooling the suspension to be synthesized to normal temperature, centrifugally separating for 1min at 8000rpm, washing for 5 times by using distilled water and absolute ethyl alcohol, and drying to obtain high-purity NaVO 2 The electrode material 6 of the nanoparticle.
Comparative example 1 of example 1: zheng Chuanli A new technological study [ D ] of preparing vanadium oxide by reducing sodium metavanadate, hebei university of science and technology, 2015, comprises the following experimental steps: accurately weighing about 20g of sodium metavanadate in a material boat, wherein the material layer is 1.Scm thick, placing the material boat in an isothermal zone of a heat-resistant stainless steel tube of a tube furnace, connecting a gas inlet and outlet pipeline, introducing nitrogen to displace air in a reduction system, heating up after setting heating up time and reduction time for 3 hours by a program temperature controller, heating up to 700 ℃, replacing nitrogen in a gas channel with hydrogen to start reduction reaction, replacing hydrogen with nitrogen after the reduction reaction is finished, naturally cooling along with the furnace or taking the heat-resistant stainless steel tube out of the tube furnace to forcibly cool down, closing the gas channel after cooling to normal temperature, taking out the material boat, performing multiple room temperature water slurrying washing on the obtained product until the pH value of the obtained filtrate is close to neutral, and respectively analyzing the contents of vanadium, sodium and alkali after the volume of the obtained filtrate is fixed. And (5) after the filter cake is dried, determining the content of vanadium and sodium in the solid phase. The conversion rate of vanadium in the reduction reaction process can be calculated by analyzing the unreduced pentavalent vanadium in the filtrate.
The method prepares NaVO by hydrogen reduction 2 The method has the defects of complex operation, high energy consumption and low repeatability, and the obtained product is impure and uncontrollable in morphology.
The patent discloses a controllable preparation method of NaVO 2 A method for preparing a nanosphere sodium storage electrode material; the method is characterized in that: accurately weigh 10.0000g of analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh; mixing the above two materials for 20min, and adding the mixture into 100 mlA stainless steel ball grinding tank, wherein the diameter of a stainless steel grinding ball is 5mm, the ball-material ratio is regulated and controlled to be 1:1, the rotating speed of a planetary ball mill is regulated and controlled to be 100rpm, the grinding mixing temperature is controlled to be 50 ℃, the interval time between the forward rotation and the reverse rotation of the ball mill is 15 minutes, the total ball milling time is 2 hours, and the ball milling tank and uniform powder materials are separated; and then controlling the vertical pressure to be 10MPa and the constant pressure to be 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining the precursor compact with the thickness of 4mm and the diameter of 10 mm. Placing the precursor compacting sheet in a muffle furnace for sintering in an air environment, wherein the heat treatment heating order is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; and then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color. Grinding 0.5000g of the pure phase material into powder of 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to be 200 watts, reacting at 100 ℃ for 4 hours, cooling the suspension to be synthesized, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 3-5 times, and drying to obtain high-purity NaVO 2 Nanoparticle electrode material 1.
Claims (1)
1. Controllable NaVO preparation 2 A method for preparing a nanosphere sodium storage electrode material; naVO with regular morphology and uniform size can be prepared by controlling the reaction parameter conditions 2 Nanosphere sodium storage electrode material; in the experiment, the two methods of high-temperature sintering and microwave radiation are combined, so that the operation process is simplified, the preparation cost is reduced, the purity of the product is improved, the repeatability of the reaction is improved, and the NaVO is realized 2 The mass production of the nanosphere sodium storage electrode material has significance;
in order to achieve the above purpose, the present invention uses the following technical scheme:
first, accurately weigh 10.0000g analytically pure V 2 O 5 A powder having a powder particle size of 200 mesh; simultaneously accurately weighing analytically pure Na 2 CO 3 5.8275g of (2) having a mesh size of 200 mesh;
secondly, fully and uniformly mixing the two materials for 20min, adding the mixed material into a stainless steel ball grinding tank with the volume of 100 ml, adding stainless steel grinding balls with the diameter of 5mm, regulating the ball-material ratio to be 1:1, regulating the rotating speed of a planetary ball mill to be 100rpm, controlling the mixing temperature of grinding to be 40-50 ℃, controlling the interval time between forward rotation and reverse rotation of the ball mill to be 15 min, and separating the ball grinding tank and uniform powder materials for 2 h;
thirdly, controlling the vertical pressure to be 10-15 MPa for 50 seconds by using a tabletting die with the diameter of 10mm, and finally obtaining a precursor compact sheet with the thickness of 4-5 mm and the diameter of 10 mm;
fourthly, placing the precursor compacting sheet obtained in the previous step in a muffle furnace for sintering in an air environment, wherein the heat treatment heating order is as follows: gradually heating from room temperature to 550 ℃, wherein the heating rate is 10 ℃/min, and the constant-temperature heating time at 550 ℃ lasts for 3 hours; then continuously heating to 900 ℃ and sintering for 5 hours at constant temperature to obtain pure phase materials with uniform color and luster;
fifthly, grinding 0.5000g of the pure phase material into powder to 200 meshes in a mortar, adding the powder into a 150 ml quartz round-bottom flask of a microwave reactor with a reflux cooling device at normal pressure, adding 50.0ml of distilled water into the round-bottom flask, controlling the radiation power to be 200-1500 watts, and heating the system for 4 hours at the reaction temperature of 100 ℃;
sixthly, cooling the suspension to be synthesized to normal temperature, centrifuging at 8000rpm for 1min, washing with distilled water and absolute ethyl alcohol for 3-5 times, and drying to obtain high-purity NaVO 2 An electrode material of the nanoparticle; the NaVO 2 The shape of the nano particles is spherical, and the particle size is 50-200 nm; the NaVO 2 The nanosphere sodium storage electrode material is used as an electrode material of a sodium ion battery.
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