CN108996557B - Hollow sphere structured nickel oxide/copper oxide composite nano material and preparation method thereof - Google Patents
Hollow sphere structured nickel oxide/copper oxide composite nano material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nickel oxide/copper oxide composite nano material with a hollow sphere structure and a preparation method thereof, wherein the preparation method comprises the following steps: dissolving nickel salt and cupric salt in a solvent to obtain a mixed solution, sequentially adding a high-molecular auxiliary reagent and urea into the mixed solution, stirring until the nickel salt and the cupric salt are completely dissolved, then carrying out hydrothermal reaction, further calcining the obtained product, and obtaining the nickel oxide/copper oxide composite nano material with the hollow sphere structure after the calcination is finished. Compared with the prior art, the method has the advantages of cheap and easily-obtained raw materials, no need of additionally adding a template in a reaction system for obtaining the hollow structure, simple synthesis process, controllable structure and size of the obtained product and high product yield.
Description
Technical Field
The invention belongs to the technical field of preparation processes of inorganic micro-nano materials, and particularly relates to a nickel oxide/copper oxide composite nano material with a hollow sphere structure and a preparation method thereof.
Background
The inorganic oxide hollow micro-nano material has the advantages of low density, high specific surface area, high permeability, high thermal stability, high thermodynamic stability and the like due to the characteristics of the hollow structure, shows wide application prospects in the fields of catalysis, adsorption and gas sensitivity, energy and energy, medicine storage and release and the like in recent years, and can be used in the fields of light material additives, sound insulation and heat insulation materials, medicine slow release carriers, catalyst carriers and the like; the oxide hollow sphere has excellent performances such as high yield and high specific surface area, so that the oxide hollow sphere has great application prospects in the physical and chemical fields such as electricity, magnetism, adsorption, catalysis and the like.
From the viewpoint of the inherent properties of materials, the performance of a single metal oxide, such as CuO, as a P-type semiconductor, is poor, which affects the application of the P-type semiconductor as an electrochemical material. Therefore, the combination of various metal oxides can make up the performance deficiency of the oxide material with single component, so that the material has better application effect in the electrochemical fields of electrocatalysis, battery electrodes and the like.
By preparing the inorganic oxide material into a hollow micro-nano structure and carrying out a series of regulation and control on the composition, morphology, size and the like of the oxide material with the hollow micro-nano structure, specific functions and attributes can be given to the material, so that the material has the characteristics superior to those of conventional oxide material powder particles in different aspects such as mechanics, electricity, optics and the like.
Therefore, different inorganic oxides are combined with each other and further prepared into the composite nano material with the hollow micro-nano structure, which is an effective means for improving the material performance, such as improving the catalytic performance of a photoelectric catalyst, improving the sensitivity and the recovery capability of a gas sensor, improving the electrochemical performance of an electrode material and the like. At present, the template method is the most common method for preparing hollow-structure micro-nano materials. The method comprises the following steps: firstly, synthesizing a template, depositing or coating a target product on the surface of the template, and then removing the template inside to obtain a hollow structure material; or a prepared template is taken as a reactant, reaction is carried out on the surface of the template, and a hollow structure is formed in the template based on the kirkendall effect. The template method for preparing the hollow-structure micro-nano material has the defects of complicated process and high production cost, so that the practical application and popularization of the hollow-structure micro-nano material are limited.
Therefore, a method with simple process and low cost is found, and the preparation of the hollow-structure micro-nano material, especially the preparation of the hollow-structure composite micro-nano material is necessary, so that more scientific bases and technical supports are provided for the application and development of the micro-nano material.
Disclosure of Invention
The invention aims to provide the nickel oxide/copper oxide composite nanomaterial with the hollow sphere structure and the preparation method thereof.
The invention provides a preparation method of a nickel oxide/copper oxide composite nano material with a hollow sphere structure, which comprises the following steps:
A. dissolving a nickel salt and a cupric salt in a solvent to obtain a solution a;
B. sequentially adding a polymer auxiliary reagent and urea into the solution a formed in the step A, and stirring until the polymer auxiliary reagent and the urea are completely dissolved to obtain a solution b;
C. carrying out hydrothermal reaction on the solution b, separating the solution from the product after the reaction is finished, and further cleaning and drying the product obtained by separation;
D. and C, further calcining the dried product obtained in the step C, and obtaining the nickel oxide/copper oxide composite nano material with the hollow sphere structure after the calcination is finished.
In the step A, the nickel salt is one or more of nitrate, sulfate, chloride and acetate of nickel containing crystal water or not containing crystal water; the cupric salt is one or more of nitrate, sulfate, chloride and acetate of cupric salt containing or not containing crystal water.
Further, in step a, the nickel salt and the cupric salt are preferably nickel nitrate hexahydrate and copper nitrate trihydrate, respectively.
In step A, Ni in the nickel salt and the cupric salt2+、Cu2+The amount of (a) is 1:1 to 1.5, Ni2+The concentration in the solvent is 20-27 mmol/L.
In the step A, the solvent is deionized water or a mixed solution of deionized water and ethylene glycol according to a volume ratio of 1-2: 1.
In the step B, the ratio of the polymer auxiliary reagent, the urea and the solvent in the step A is 13-40 g: 16-25 g: 1L of the compound.
In the step B, the polymer auxiliary reagent is polyvinylpyrrolidone; polyvinylpyrrolidone with a K value of 30 is preferred.
In the step C, the temperature and the time of the hydrothermal reaction are respectively 80-140 ℃ and 8-12 hours; preferably 90 ℃ for 10 hours.
In the step D, the calcining is carried out for 3-5 hours after the temperature is raised from room temperature to 700-800 ℃ in the air atmosphere.
The invention also provides the nickel oxide/copper oxide composite nano material with the hollow sphere structure prepared by the preparation method, and the size of the prepared nickel oxide/copper oxide composite nano material with the hollow sphere structure can be effectively regulated and controlled by regulating the component ratio of the solvent.
In the method for preparing the nickel oxide/copper oxide composite nano material with the hollow sphere structure, the existence of the high-molecular auxiliary reagent polyvinylpyrrolidone increases the viscosity of the reaction liquid, so that gas generated by urea decomposition in the reaction heating process forms bubbles in the reaction liquid. The polyvinylpyrrolidone molecules are gathered on the surfaces of the bubbles, so that the bubbles stably exist in the reaction liquid. Since the unbound electrons on O and N on the polyvinylpyrrolidone chain can form coordinate bonds with the metal ions, this allows the metal ions to also aggregate on the surface of the bubbles. Under hydrothermal conditions, the metal ions further react with OH in water-And reacting to generate hydroxide precipitate on the surface of the bubbles, thereby forming a hollow sphere structure. And (3) converting the hydroxide into an oxide through subsequent calcination, and finally obtaining the nickel oxide/copper oxide composite nano material with the hollow sphere structure. The addition of the dihydric alcohol in the solvent can further increase the viscosity of the reaction system, so that bubbles formed by the gas after urea decomposition are not easy to gather, and the bubbles with smaller sizes are obtained. Therefore, the size of the prepared nickel oxide/copper oxide composite nano-material with the hollow sphere structure is effectively regulated and controlled by adjusting the proportion of the dihydric alcohol in the solvent.
According to the method for preparing the nickel oxide/copper oxide composite nano material with the hollow sphere structure, the hollow micro-nano structure is obtained without additionally adding a hard template, the prepared material is uniform in size, uniform in structure, simple in process, good in reproducibility, simple in reaction device, cheap and easily available in reaction materials, low in preparation cost and easy to amplify, and large-scale production is realized. The prepared material is a composite material formed by two metal oxides, and the performance is improved compared with that of a single metal oxide nano material; and the hollow sphere structure has the advantages of large specific surface area, small density and the like. Therefore, the nickel oxide/copper oxide composite nano material with the hollow sphere structure provided by the preparation method can be applied to various fields such as electrocatalysis, electrode materials of super capacitors, electrode materials of Li-ion batteries and the like.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of a nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure prepared in example 1 of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a hollow sphere structured nickel oxide/copper oxide composite nanomaterial prepared in example 1 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of a hollow sphere structured nickel oxide/copper oxide composite nanomaterial prepared in example 2 of the present invention;
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of a hollow sphere structured nickel oxide/copper oxide composite nanomaterial prepared in example 3 of the present invention;
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of a hollow sphere structured nickel oxide/copper oxide composite nanomaterial prepared in example 4 of the present invention;
FIG. 6 is a Scanning Electron Microscope (SEM) photograph of a hollow sphere structured nickel oxide/copper oxide composite nanomaterial prepared in example 5 of the present invention;
fig. 7 is a Scanning Electron Microscope (SEM) photograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure prepared in example 6 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings.
Example 1
A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure comprises the following steps:
A. weighing 0.8mmol of nickel nitrate hexahydrate and 0.8mmol of copper nitrate trihydrate, adding the nickel nitrate hexahydrate and the copper nitrate trihydrate into 30mL of mixed solution formed by deionized water and ethylene glycol according to the volume ratio of 2:1, and stirring until the nickel nitrate hexahydrate and the copper nitrate trihydrate are completely dissolved to obtain clear and transparent solution;
B. adding 0.48g of urea and 1.2g of polyvinylpyrrolidone into the solution obtained in the step A, and stirring until the urea and the polyvinylpyrrolidone are completely dissolved to obtain a clear and transparent mixed solution;
C. and D, transferring the mixed solution obtained in the step B into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a constant temperature box, reacting for 10 hours at the constant temperature of 90 ℃, and cooling to room temperature. Centrifuging the liquid cooled in the reaction kettle to separate a solid product, washing and centrifuging the product by using alcohol, washing and centrifuging the product by using ultrapure water, repeating the operation for 2 times, placing the obtained solid product in a drying box, and drying the solid product for 6 hours at the temperature of 90 ℃;
D. and D, placing the solid product dried in the step C in a muffle furnace, heating to 700 ℃ at room temperature in the air atmosphere, calcining for 3 hours, and naturally cooling to room temperature to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure.
FIG. 1 shows the X-ray diffraction pattern of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 1. As can be seen from FIG. 1, the positions of the diffraction peaks of the obtained material coincide with those of nickel oxide cards 47 to 1049 and copper oxide cards 45 to 0937 of JCPDS (Joint Committee for powder diffraction standards), indicating that the product is a composite material composed of nickel oxide and copper oxide.
FIG. 2 is a scanning electron micrograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 1, showing that the material has a spherical structure composed of particles, and the average sphere diameter is 600 nm. Through the opening on the surface of the obtained spherical material, the structural characteristic that the interior of the material is hollow can be observed.
Example 2
A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure comprises the following steps:
A. weighing 0.8mmol of nickel nitrate hexahydrate and 0.8mmol of copper nitrate trihydrate, adding the nickel nitrate hexahydrate and the copper nitrate trihydrate into 30mL of deionized water, and stirring until the nickel nitrate hexahydrate and the copper nitrate trihydrate are completely dissolved to obtain a clear and transparent solution;
B. adding 0.48g of urea and 1.2g of polyvinylpyrrolidone into the solution obtained in the step A, and stirring until the urea and the polyvinylpyrrolidone are completely dissolved to obtain a clear and transparent mixed solution;
C. and D, transferring the mixed solution obtained in the step B into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a constant temperature box, reacting for 8 hours at the constant temperature of 120 ℃, and cooling to room temperature. Centrifuging the liquid cooled in the reaction kettle to separate a solid product, washing and centrifuging the product by using alcohol, washing and centrifuging the product by using ultrapure water, repeating the operation for 2 times, placing the obtained solid product in a drying box, and drying the solid product for 6 hours at the temperature of 90 ℃;
D. and D, placing the solid product dried in the step C in a muffle furnace, heating to 700 ℃ at room temperature in the air atmosphere, calcining for 4 hours, and naturally cooling to room temperature to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure.
FIG. 3 is a scanning electron micrograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 2, which shows that the material has a spherical structure composed of particles, and the average sphere diameter is 900 nm. Through the opening on the surface of the obtained spherical material, the structural characteristic that the interior of the material is hollow can be observed.
Example 3
A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure comprises the following steps:
A. weighing 0.8mmol of nickel nitrate hexahydrate and 0.8mmol of copper nitrate trihydrate, adding the nickel nitrate hexahydrate and the copper nitrate trihydrate into 40mL of mixed solution formed by deionized water and ethylene glycol in a volume ratio of 1:1, and stirring until the mixed solution is completely dissolved to obtain clear and transparent solution;
B. adding 1.0g of urea and 0.8g of polyvinylpyrrolidone into the solution obtained in the step A, and stirring until the urea and the polyvinylpyrrolidone are completely dissolved to obtain a clear and transparent mixed solution;
C. and D, transferring the mixed solution obtained in the step B into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a constant temperature box, reacting for 12 hours at the constant temperature of 70 ℃, and cooling to room temperature. Centrifuging the liquid cooled in the reaction kettle to separate a solid product, washing and centrifuging the product by using alcohol, washing and centrifuging the product by using ultrapure water, repeating the operation for 2 times, placing the obtained solid product in a drying box, and drying the solid product for 6 hours at the temperature of 80 ℃;
D. and D, placing the solid product dried in the step C in a muffle furnace, heating to 700 ℃ at room temperature in the air atmosphere, calcining for 4 hours, and naturally cooling to room temperature to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure.
FIG. 4 is a scanning electron micrograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 3, showing that the material has a spherical structure composed of particles, and the average sphere diameter is 1200 nm. Through the opening on the surface of the obtained spherical material, the structural characteristic that the interior of the material is hollow can be observed.
Example 4
A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure comprises the following steps:
A. weighing 0.8mmol of nickel nitrate hexahydrate and 1.2mmol of copper nitrate trihydrate, adding the nickel nitrate hexahydrate and the copper nitrate trihydrate into 35mL of mixed solution formed by deionized water and ethylene glycol in a volume ratio of 1.33:1, and stirring until the nickel nitrate hexahydrate and the copper nitrate trihydrate are completely dissolved to obtain clear and transparent solution;
B. adding 0.6g of urea and 1.2g of polyvinylpyrrolidone into the solution obtained in the step A, and stirring until the urea and the polyvinylpyrrolidone are completely dissolved to obtain a clear and transparent mixed solution;
C. transferring the mixed solution obtained in the step B into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a constant temperature box, reacting for 6 hours at the constant temperature of 140 ℃, cooling to room temperature, centrifugally separating the liquid cooled in the reaction kettle to obtain a solid product, washing and centrifuging the product with alcohol, washing and centrifuging the product with ultrapure water, repeating the operation for 2 times, placing the obtained solid product into a drying box, and drying for 6 hours at the temperature of 90 ℃;
D. and D, placing the solid product dried in the step C in a muffle furnace, heating to 700 ℃ at room temperature in the air atmosphere, calcining for 5 hours, and naturally cooling to room temperature to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure.
FIG. 5 is a scanning electron micrograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 4, which shows that the material has a spherical structure composed of particles, and the average sphere diameter is 900 nm. Through the opening on the surface of the obtained spherical material, the structural characteristic that the interior of the material is hollow can be observed.
Example 5
A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure comprises the following steps:
A. 0.8mmol of nickel nitrate hexahydrate and 0.96mmol of copper nitrate trihydrate are weighed, the nickel nitrate hexahydrate and the copper nitrate trihydrate are added into 30mL of mixed solution formed by deionized water and ethylene glycol in a volume ratio of 2:1, and the mixed solution is stirred until the nickel nitrate hexahydrate and the copper nitrate trihydrate are completely dissolved to obtain clear and transparent solution. The volume ratio of the amount of Ni ion substances in the obtained solution to the solvent is 26.7 mol/L;
B. adding 0.6g of urea and 0.4g K of polyvinylpyrrolidone into the solution obtained in the step A, and stirring until the urea and the polyvinylpyrrolidone are completely dissolved to obtain a clear and transparent mixed solution;
C. and D, transferring the mixed solution obtained in the step B into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a constant temperature box, reacting for 12 hours at the constant temperature of 60 ℃, and cooling to room temperature. Centrifuging the liquid cooled in the reaction kettle to separate a solid product, washing and centrifuging the product by using alcohol, washing and centrifuging the product by using ultrapure water, repeating the operation for 2 times, placing the obtained solid product in a drying box, and drying the solid product for 6 hours at the temperature of 90 ℃;
D. and D, placing the solid product dried in the step C in a muffle furnace, heating to 800 ℃ at room temperature in the air atmosphere, calcining for 3 hours, and naturally cooling to room temperature to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure.
FIG. 6 is a scanning electron micrograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 5, showing that the material has a spherical structure composed of particles, and the average sphere diameter is 800 nm. Through the opening on the surface of the obtained spherical material, the structural characteristic that the interior of the material is hollow can be observed.
Example 6
A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure comprises the following steps:
A. weighing 0.8mmol of nickel acetate tetrahydrate and 0.8mmol of copper acetate monohydrate, adding the nickel acetate tetrahydrate and the copper acetate monohydrate into 30mL of mixed solution formed by deionized water and ethylene glycol in a volume ratio of 2:1, and stirring until the mixed solution is completely dissolved to obtain clear and transparent solution;
B. adding 0.6g of urea and 0.8g of polyvinylpyrrolidone into the solution obtained in the step A, and stirring until the urea and the polyvinylpyrrolidone are completely dissolved to obtain a clear and transparent mixed solution;
C. and D, transferring the solution obtained in the step B into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, placing the reaction kettle into a constant temperature box, reacting for 10 hours at the constant temperature of 90 ℃, and cooling to room temperature. Centrifuging the liquid cooled in the reaction kettle to separate a solid product, washing and centrifuging the product by using alcohol, washing and centrifuging the product by using ultrapure water, repeating the operation for 2 times, placing the obtained solid product in a drying box, and drying the solid product for 6 hours at the temperature of 90 ℃;
D. and D, placing the solid product dried in the step C in a muffle furnace, heating to 700 ℃ at room temperature in the air atmosphere, calcining for 5 hours, and naturally cooling to room temperature to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure.
FIG. 7 is a scanning electron micrograph of the nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure obtained in example 6, showing that the material has a spherical structure composed of particles, and the average sphere diameter is 600 nm. Through the opening on the surface of the obtained spherical material, the structural characteristic that the interior of the material is hollow can be observed.
The above detailed description of the nickel oxide/copper oxide composite nanomaterial with hollow sphere structure and the method for preparing the same with reference to the embodiments is illustrative and not restrictive, and several embodiments can be enumerated according to the limited scope, so that changes and modifications without departing from the general concept of the present invention shall fall within the protection scope of the present invention.
Claims (7)
1. A preparation method of nickel oxide/copper oxide composite nano-material with a hollow sphere structure is characterized by comprising the following steps:
A. dissolving a nickel salt and a cupric salt in a solvent to obtain a solution a;
B. sequentially adding a polymer auxiliary reagent and urea into the solution a formed in the step A, and stirring until the polymer auxiliary reagent and the urea are completely dissolved to obtain a solution b;
C. transferring the solution b into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, carrying out hydrothermal reaction, separating the solution from a product after the reaction is finished, and further cleaning and drying the product obtained by separation;
D. c, further calcining the dried product obtained in the step C to obtain the nickel oxide/copper oxide composite nano material with the hollow sphere structure after the calcination is finished;
in the step B, the polymer auxiliary reagent is polyvinylpyrrolidone;
in the step C, the temperature and the time of the hydrothermal reaction are respectively 80-140 ℃ and 8-12 hours;
in the step D, the calcining is carried out for 3-5 hours after the temperature is raised to 700-800 ℃ from the room temperature.
2. The preparation method according to claim 1, wherein in step a, the nickel salt is one or more of nitrate, sulfate, chloride and acetate of nickel containing or not containing crystal water; the cupric salt is one or more of nitrate, sulfate, chloride and acetate of cupric salt containing or not containing crystal water.
3. The method according to claim 1 or 2, wherein in step a, the nickel salt and the cupric salt are nickel nitrate hexahydrate and copper nitrate trihydrate, respectively.
4. The method according to claim 1, wherein in step A, Ni is contained in the nickel salt and the cupric salt2 +、Cu2+The amount of (a) is 1:1 to 1.5, Ni2+The concentration in the solvent is 20-27 mmol/L.
5. The preparation method according to claim 1 or 4, wherein in the step A, the solvent is deionized water or a mixed solution of deionized water and ethylene glycol according to a volume ratio of 1-2: 1.
6. The preparation method according to claim 1, wherein in the step B, the ratio of the polymeric auxiliary reagent to the urea to the solvent in the step A is 13-40 g: 16-25 g: 1L of the compound.
7. The nickel oxide/copper oxide composite nanomaterial with a hollow sphere structure prepared by the preparation method according to any one of claims 1 to 6.
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| CN115634693B (en) * | 2022-09-30 | 2024-01-26 | 惠州学院 | Preparation method of nanocomposite with hollow tube structure and application of nanocomposite in catalyzing aminoborane alcoholysis to produce hydrogen |
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