阅读说明：本技术 一种纳米氧化锌-氧化钒复合材料的制备方法 (Preparation method of nano zinc oxide-vanadium oxide composite material ) 是由 刘艺 于 2020-05-26 设计创作，主要内容包括：本发明涉及新材料加工技术领域,公开了一种纳米氧化锌-氧化钒复合材料的制备方法,利用简单的水热反应法得到氧化锌纳米片,分散到钒酸铵盐溶液中,煅烧制备得到具有特殊结构和形貌的纳米氧化锌-氧化钒复合材料,粒径在30-35纳米范围均匀分布,具有极好的电磁活性,将其应用于电容器领域,不仅具有较大的电容容量,还表现出优异的可逆性,避免了纳米电极材料稳固性差、易脱落,降低电极可逆性等带来的相应问题；采用本发明制备得到的纳米氧化锌-氧化钒复合材料制备复合电极,进行电化学测试,测定本发明制备得到的复合材料的电化学性能,试验表明,当电流密度为1mA/g时,该材料的电极比容量达到了276-282F/g。(The invention relates to the technical field of new material processing, and discloses a preparation method of a nano zinc oxide-vanadium oxide composite material, wherein a simple hydrothermal reaction method is utilized to obtain zinc oxide nano sheets, the zinc oxide nano sheets are dispersed into an ammonium vanadate solution, and the nano zinc oxide-vanadium oxide composite material with a special structure and morphology is prepared by calcining, the particle size is uniformly distributed in the range of 30-35 nanometers, the nano zinc oxide-vanadium oxide composite material has excellent electromagnetic activity, and the nano zinc oxide-vanadium oxide composite material is applied to the field of capacitors, has larger capacitance capacity and excellent reversibility, avoids the corresponding problems caused by poor stability, easy falling, reduced electrode reversibility and the like of a nano electrode material; the composite electrode prepared from the nano zinc oxide-vanadium oxide composite material prepared by the invention is used for electrochemical test, and the electrochemical performance of the composite material prepared by the invention is measured, and the test shows that when the current density is 1mA/g, the electrode specific capacity of the material reaches 276-282F/g.)

1. A preparation method of a nano zinc oxide-vanadium oxide composite material is characterized by comprising the following steps:

(1) weighing 12.5-13.0 g of zinc nitrate, placing the zinc nitrate into a beaker, adding deionized water into the beaker under the stirring of the speed of 300-350 r/min, continuously stirring until the zinc nitrate is dissolved, preparing a zinc nitrate solution with the molar concentration of 0.35-0.40 mol/l, dropwise adding a sodium hydroxide solution into the beaker at the temperature of 45-50 ℃, adjusting the pH value of the system to be 8.1-8.2, and stirring the mixture for 15-20 min under a magnetic stirrer to obtain a solid-liquid mixture;

(2) continuously stirring the solid-liquid mixture obtained in the step (1) for 15-20 minutes at 220 revolutions per minute, transferring the mixture into a hydrothermal reaction kettle, reacting for 16-18 hours at 180 ℃, taking out the reaction kettle, placing the reaction kettle in a fume hood, naturally cooling to room temperature, removing a product, washing the obtained product with ethanol and deionized water for 3-5 times respectively, placing the product in a drying oven at 75-80 ℃ for drying for 8-10 hours, then placing the product in a muffle furnace for calcining for 70-80 minutes at 360 ℃ to obtain a zinc oxide nanosheet;

(3) weighing 9.8-10.0 g of sodium metavanadate, adding the sodium metavanadate into 60-75 ml of hot water at the temperature of 60-65 ℃ to dissolve the sodium metavanadate under stirring, then adding 10-12 ml of polyethylene glycol aqueous solution with the mass concentration of 26-30%, stirring the mixture for 10-15 minutes at the speed of 500-550 revolutions/minute, weighing 1.32-1.36 g of ammonium oxalate, adding the ammonium oxalate into the solution, and continuously and quickly stirring the mixture for 30-40 minutes to obtain an ammonium vanadate solution;

(4) adding the zinc oxide nano-sheet prepared in the step (2) into the ammonium vanadate solution prepared in the step (3), adding 23-25 ml of deionized water for dilution, continuously stirring for 15-20 minutes at the speed of 350 revolutions per minute of 300-, placing the mixture in a 180-190 ℃ forced air drying box, carrying out pressurized reaction for 13-16 hours, the reaction pressure is 1.35-1.40MPa, when the reaction kettle is naturally cooled to 20-25 ℃, pouring out supernatant liquor, centrifugally washing the precipitate for 4-6 times by using deionized water and absolute ethyl alcohol in sequence, then placing the product in an oven at 70-80 ℃ for drying for 10-14 hours, then putting the mixture into a muffle furnace to be calcined for 1.5 to 2.0 hours at the calcining temperature of 420-430 ℃, and naturally cooling to obtain the nano zinc oxide-vanadium oxide composite material.

2. The method for preparing nano zinc oxide-vanadium oxide composite material according to claim 1, wherein the molar concentration of the sodium hydroxide solution in the step (1) is 2.7-3.0 mol/l.

3. The method for preparing the nano zinc oxide-vanadium oxide composite material according to claim 1, wherein the muffle furnace calcination temperature rise speed in the step (2) is 6.6-7.0 ℃/min.

4. The method for preparing the nano zinc oxide-vanadium oxide composite material according to claim 1, wherein the zinc oxide nano-sheets prepared in the step (2) have a particle size of 10 to 25 nm.

5. The method for preparing nano zinc oxide-vanadium oxide composite material according to claim 1, wherein the polyethylene glycol aqueous solution in the step (3) is prepared from polyethylene glycol with molecular weight of 400.

6. The method for preparing nano zinc oxide-vanadium oxide composite material according to claim 1, wherein the nano zinc oxide-vanadium oxide composite material prepared in the step (4) has a particle size of 30-35 nm.

Technical Field

The invention belongs to the technical field of new material processing, and particularly relates to a preparation method of a nano zinc oxide-vanadium oxide composite material.

Background

The nano zinc oxide refers to zinc oxide particles with the grain size of below 100 nanometers, and as a high-performance semiconductor material, the nano zinc oxide shows a plurality of special properties such as non-toxicity, non-migration, fluorescence, piezoelectricity, ultraviolet absorption and scattering capacity and the like due to the unique small-size effect, surface effect, quantum size effect, macroscopic quantum tunneling effect and dielectric confinement effect. Therefore, the nano-material has wide application prospect in the fields of antibacterial materials, luminescent materials, piezoelectric materials, ultraviolet shielding materials, self-cleaning materials, cell calibration materials, nano-catalysts and the like.

Due to synergistic effect and other effects in the preparation of the nano composite material, the composite material shows one or more new functions which are often not possessed by the original substance, and the appearance of the new functions opens up a new application field of the nano material. Due to its superior performance and wide application prospect, it is one of the hot spots in the current scientific research of nano materials. At present, the research on the nano zinc oxide in the technical field of electromagnetic functions is not yet mature, the nano zinc oxide is not applied well basically, and a huge development space exists.

Disclosure of Invention

The invention aims to solve the existing problems and provides a preparation method of a nano zinc oxide-vanadium oxide composite material, wherein zinc oxide nano sheets are obtained by a simple hydrothermal reaction method, dispersed into an ammonium vanadate solution, and calcined to obtain the nano zinc oxide-vanadium oxide composite material with a special structure and morphology, the particle size is uniformly distributed in the range of 30-35 nanometers, and the nano zinc oxide-vanadium oxide composite material has excellent electromagnetic activity.

The invention is realized by the following technical scheme:

a preparation method of a nano zinc oxide-vanadium oxide composite material has the preferred scheme that,

(1) weighing 12.5-13.0 g of zinc nitrate, placing the zinc nitrate into a beaker, adding deionized water into the beaker under the stirring of the speed of 300-350 r/min, continuously stirring until the zinc nitrate is dissolved, preparing to obtain a zinc nitrate solution with the molar concentration of 0.35-0.40 mol/l, dropwise adding a sodium hydroxide solution with the molar concentration of 2.7-3.0 mol/l into the beaker at the temperature of 45-50 ℃, adjusting the pH value of the system to be 8.1-8.2, and stirring for 15-20 minutes under a magnetic stirrer to obtain a solid-liquid mixture;

(2) continuously stirring the prepared solid-liquid mixture for 15-20 minutes at 220 revolutions per minute of 200-;

(3) weighing 9.8-10.0 g of sodium metavanadate, adding the sodium metavanadate into 60-75 ml of hot water at the temperature of 60-65 ℃ to dissolve the sodium metavanadate under stirring, then adding 10-12 ml of polyethylene glycol aqueous solution with the mass concentration of 26-30%, stirring the mixture for 10-15 minutes at the speed of 500-550 revolutions/minute, weighing 1.32-1.36 g of ammonium oxalate, adding the ammonium oxalate into the solution, and continuously and quickly stirring the mixture for 30-40 minutes to obtain an ammonium vanadate solution; the polyethylene glycol aqueous solution is prepared from polyethylene glycol with the molecular weight of 400;

(4) adding the prepared zinc oxide nano-sheet into an ammonium vanadate solution, adding 23-25 ml of deionized water for dilution, continuously stirring for 15-20 minutes at 350 revolutions per minute of 300-25 ℃, transferring to a polytetrafluoroethylene reaction kettle, placing in a 180-190 ℃ forced air drying box, performing pressurized reaction for 13-16 hours at the reaction pressure of 1.35-1.40MPa, naturally cooling the reaction kettle to 20-25 ℃, pouring out supernatant liquid, centrifugally washing precipitates for 4-6 times by using deionized water and absolute ethyl alcohol in sequence, placing the product in a 70-80 ℃ drying box for drying for 10-14 hours, then placing in a muffle furnace for calcining for 1.5-2.0 hours at the calcining temperature of 420-430 ℃, and naturally cooling to obtain the nano zinc oxide-vanadium oxide composite material.

The particle size of the zinc oxide nano-sheet prepared by the hydrothermal reaction method is between 10 and 25 nanometers.

The grain size of the prepared nano zinc oxide-vanadium oxide composite material is between 30 and 35 nanometers.

Compared with the prior art, the invention has the following advantages: in order to solve the problem that the existing nano zinc oxide is still immature in research in the technical field of electromagnetic functions and cannot be well applied, the invention provides a preparation method of a nano zinc oxide-vanadium oxide composite material, a simple hydrothermal reaction method is utilized to obtain zinc oxide nano sheets, the zinc oxide nano sheets are dispersed into an ammonium vanadate salt solution, and the nano zinc oxide-vanadium oxide composite material with a special structure and appearance is prepared by calcining, the particle size is uniformly distributed in the range of 30-35 nanometers, the nano zinc oxide-vanadium oxide composite material has excellent electromagnetic activity, and the nano zinc oxide-vanadium oxide composite material is applied to the field of capacitors, has larger capacitance capacity and excellent reversibility, and avoids the corresponding problems caused by poor stability, easy falling, reduced electrode reversibility and the like of a nano electrode material; the composite electrode prepared from the nano zinc oxide-vanadium oxide composite material prepared by the method is used for carrying out electrochemical test, and the electrochemical performance of the composite material prepared by the method is measured, wherein the test shows that when the current density is 1mA/g, the electrode specific capacity of the material reaches 276-282F/g; the invention can obviously improve the electromagnetic activity of the nano zinc oxide composite material and solve the problem of poor application effect of the existing nano zinc oxide in the field of electromagnetic function. The nano zinc oxide-vanadium oxide composite material prepared by the invention has very excellent electromagnetic performance, can be applied to the aspects of solar batteries, super capacitors and the like by combining with the electronic structure of the semiconductor catalyst of the nano zinc oxide-vanadium oxide composite material, becomes a multifunctional material with huge potential, is beneficial to improving the application value of the nano zinc oxide composite material in the electromagnetic field, and is a technical scheme which is extremely worthy of popularization and use.

Detailed Description

In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described with reference to specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the present invention and are not used for limiting the technical solutions provided by the present invention.