CN109261156B - Nickel film and zinc oxide nanorod composite material as well as preparation method and application thereof - Google Patents
Nickel film and zinc oxide nanorod composite material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of photocatalytic materials, and relates to a nickel film and zinc oxide nanorod composite material as well as a preparation method and application thereof. Firstly, a collodion film is taken as a template, a nickel film is prepared by the reduction action of potassium borohydride, and the nickel film soaked by PVP is soaked in a zinc oxide seed crystal solution for a plurality of hours to adsorb a layer of zinc oxide seed crystal. Finally, the nickel film-zinc oxide nano-rod composite material is placed in a mixed solution of zinc nitrate and HMT with a certain concentration, and hydrothermal is carried out for several hours at a low temperature, so that the nickel film-zinc oxide nano-rod composite material is obtained. The invention has the advantages of low price of raw materials, simple preparation process and easy popularization. The prepared nickel film-zinc oxide nano-rod composite material has more excellent photocatalysis performance than a pure zinc oxide nano-rod material.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a nickel film and zinc oxide nanorod composite material as well as a preparation method and application thereof.
Background
With the rapid development of the industry, a large amount of industrial wastewater is discharged into the natural environment, and the water pollution is more serious. The organic contaminants in these wastewaters are of a wide variety and a large portion are teratogenic. Therefore, how to solve the pollution problem in the water body becomes one of the problems to be solved urgently at present.
Zinc oxide photocatalysis is a novel photocatalysis technology, and is widely applied to sewage treatment because of the characteristics of mild preparation conditions, no secondary pollution, good chemical stability, low price and the like. However, the zinc oxide photocatalytic material has defects, and due to the wide band gap, only the ultraviolet light part occupying a small amount of sunlight can be utilized, the visible light part in the sunlight is rarely utilized, and in addition, the problem that the recombination of photogenerated electron holes is fast exists. Therefore, how to improve the photocatalytic efficiency of zinc oxide becomes a research hotspot of photocatalytic technology.
The nickel film is a novel two-dimensional material, and can be prepared by directly reducing a nickel chloride solution by a chemical oxidation-reduction method by virtue of the template effect of a collodion film, and the material has a large specific surface area, abundant surface active sites and excellent conductivity. The nickel film is compounded with the zinc oxide, so that photoproduction electrons generated by the zinc oxide can be accelerated to be transferred to the surface of the nickel film, the compounding of photoproduction electron hole pairs is prevented, meanwhile, the huge specific surface area of the nickel film can enhance the adsorption performance of the material, and the degradation efficiency of the material is further improved.
Disclosure of Invention
The invention aims to provide a nickel film and zinc oxide nanorod composite material capable of improving the photocatalytic efficiency of zinc oxide, and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a nickel film and zinc oxide nanorod composite material comprises the following steps:
(A) dropping collodion liquid into a clean and dry glass culture dish, rotating to uniformly disperse the collodion liquid, naturally drying the collodion liquid to obtain a collodion film, and taking off the collodion film for later use;
(B) NiCl injected into the culture dish2·6H2O aqueous solution, sealed with the collodion film prepared in step (A), then inverted and inserted perpendicularly into the container containing KBH4After reacting for about 24 hours at room temperature in the culture dish containing the solution, the solution is filled with NiCl2·6H2A black product is generated on one side of the collodion film of the O aqueous solution; collecting the blackCentrifuging and washing the color product for several times, and drying in vacuum at 60 ℃ to obtain a nickel film;
(C) dissolving anhydrous zinc acetate in absolute ethyl alcohol, pouring into a three-neck flask, and stirring in a constant-temperature oil bath at 60 ℃ until the zinc acetate is completely dissolved; dissolving potassium hydroxide in absolute ethyl alcohol for later use; slowly dripping a potassium hydroxide solution into a zinc acetate solution under the stirring condition of a constant-temperature oil bath at 60 ℃, and heating for 2 hours under the magnetic stirring condition to obtain zinc oxide seed crystals;
(D) taking a nickel film, dispersing the nickel film in PVP solution at room temperature, magnetically stirring for 4 hours, carrying out centrifugal separation, washing the obtained solid with absolute ethyl alcohol once, and removing redundant PVP molecules; then dispersing the nickel film treated by PVP into the ZnO seed crystal solution prepared in the step (A), stirring for 3h, then carrying out centrifugal separation, washing the solid product once by using ethanol, and attaching the nickel film with ZnO seed crystals;
(E) and then dispersing the nickel film attached with the ZnO seed crystal into an aqueous solution of zinc nitrate and hexamethylenetetramine with equal molar concentration, carrying out ultrasonic dispersion, reacting for 4 hours at 90 ℃, carrying out centrifugal separation on the product, washing twice with water and ethanol respectively, and carrying out vacuum drying at 60 ℃ to obtain the nickel film and zinc oxide nanorod nanocomposite.
Further, the dropping amount of the collodion liquid in the step (A) was 7 ml.
Further, NiCl used in the step (B)2·6H2The concentration of the O aqueous solution was 5mmol/L, and the volume was 20 ml.
Further, KBH used in the step (B)4The concentration of the solution was 50mmol/L, and the volume was 20 ml.
Further, the zinc acetate solution in the step (C) was prepared by weighing 0.2294g of anhydrous zinc acetate and dissolving in 125ml of anhydrous ethanol.
Further, the potassium hydroxide solution in the step (C) was prepared by weighing 0.1094g of potassium hydroxide and dissolving in 65ml of absolute ethanol.
Further, 3mg of the nickel film was weighed in step (D) and dispersed in 20ml of 0.5g/L PVP solution.
Further, the nickel film with ZnO seed crystals in the step (E) was dispersed in 20mL of an aqueous solution of zinc nitrate and hexamethylenetetramine in equimolar concentrations, both of which were 0.004M in molar concentrations.
The invention grows zinc oxide nanometer stick on nickel film with ultrathin structure to form two-dimension array structure, the two-dimension material of nickel film is combined with one-dimension zinc oxide tightly, which transfers part of electron to nickel film, reduces electron hole recombination speed and improves catalysis property.
The invention also provides a nickel film and zinc oxide nano-rod composite material obtained by the preparation method.
The invention also provides application of the nickel film and zinc oxide nanorod composite material in degradation of rhodamine B or ciprofloxacin.
Furthermore, the nickel film and zinc oxide nanorod composite material obtained by the invention is used for degrading rhodamine B and ciprofloxacin, and the degradation experiment result shows that the nickel film and zinc oxide nanorod composite material has excellent photocatalytic performance.
Compared with the prior art, the invention has the following beneficial effects:
(1) the nickel film is prepared by adopting a chemical reduction method, and then the zinc oxide nano rod grows in situ on the nickel film through a two-step method of seed crystal adsorption and hydrothermal growth, so that the whole process is easy to operate, and the prepared composite material has good stability and has reference significance for compounding other two-dimensional materials and semiconductors.
(2) The degradation of rhodamine B and ciprofloxacin shows that the obtained nickel film and zinc oxide nanorod composite material has excellent photocatalytic performance.
Drawings
FIG. 1 is a simplified diagram of an apparatus for preparing a nickel film according to an embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of a nickel film prepared according to an example of the present invention;
FIG. 3 is a scanning electron micrograph of a nickel film and zinc oxide nanorod composite material prepared according to an embodiment of the present invention;
FIG. 4 is a transmission electron micrograph of a nickel film and zinc oxide nanorod composite material prepared according to an embodiment of the present invention;
FIG. 5 is a diagram illustrating photocatalytic degradation of a composite material of a nickel film and a zinc oxide nanorod to rhodamine B, which is prepared according to an embodiment of the present invention;
FIG. 6 is a diagram of the photocatalytic degradation of ciprofloxacin by the nickel film and zinc oxide nanorod composite material prepared in the embodiment of the invention.
Detailed Description
The invention is described in detail below with reference to the following figures and specific examples:
examples
A preparation method of a nickel film and zinc oxide nanorod composite material capable of improving the photocatalytic efficiency of zinc oxide comprises the following steps:
(A) dripping 7ml collodion solution into a clean and dry glass culture dish (specification phi 90mm), rotating to uniformly disperse the collodion solution, naturally drying the collodion solution to obtain a collodion film, and taking off the collodion film for later use; the whole process is operated in a fume hood;
(B) 20ml of 5mmol/L NiCl was poured into a petri dish (specification phi 60mm)2·6H2O aqueous solution, sealed with the collodion film prepared in step (A), then inverted and inserted vertically into a container containing 20ml of 50mmol/L KBH4After reacting for about 24 hours at room temperature in the culture dish containing the solution, the solution is filled with NiCl2·6H2A black product is generated on one side of the collodion film of the O aqueous solution; collecting the black product, centrifuging and washing for several times, and vacuum drying at 60 ℃ to obtain a nickel film;
(C) 0.2294g of anhydrous zinc acetate is weighed and dissolved in 125ml of anhydrous ethanol, the mixture is poured into a 500ml three-neck flask, and the mixture is stirred in oil bath at the constant temperature of 60 ℃ until the zinc acetate is completely dissolved; 0.1094g of potassium hydroxide is weighed and dissolved in 65ml of absolute ethyl alcohol for standby; slowly dripping a potassium hydroxide solution into a zinc acetate solution under the stirring condition of a constant-temperature oil bath at 60 ℃, and heating for 2 hours under the magnetic stirring condition to obtain zinc oxide seed crystals;
(D) weighing 3mg of nickel membrane, dispersing the nickel membrane in 20ml of 0.5g/L PVP solution at room temperature, magnetically stirring for 4 hours, carrying out centrifugal separation, washing the obtained solid with absolute ethyl alcohol once, and removing redundant PVP molecules; then dispersing the nickel film treated by PVP into the ZnO seed crystal solution prepared in the step (A), stirring for 3h, then carrying out centrifugal separation, washing the solid product once by using ethanol, and attaching the nickel film with ZnO seed crystals;
(E) and then dispersing the nickel film attached with the ZnO seed crystal into 20mL of aqueous solution of zinc nitrate (0.004M) and hexamethylenetetramine (0.004M) with the same molar concentration, performing ultrasonic dispersion, reacting for 4 hours at 90 ℃, performing centrifugal separation on a product, washing twice with water and ethanol respectively, and performing vacuum drying at 60 ℃ to obtain the nickel film and zinc oxide nanorod nanocomposite.
The nickel film and zinc oxide nano rod composite material comprises a nickel film and a zinc oxide nano rod loaded on the nickel film.
FIG. 1 is a diagram of a simple apparatus for preparing a nickel film, wherein a nickel chloride solution and a potassium borohydride solution are respectively arranged on two sides of a collodion film, after ion diffusion, a black precipitate is generated on one side of the nickel chloride solution, and after a certain reaction time, a black product is collected, washed and dried to obtain the nickel film.
Fig. 2 is a scanning electron micrograph of the prepared nickel film, and it can be seen that the prepared nickel film is relatively thin, being only several nanometers thick. And (3) adsorbing the nickel film by using zinc oxide seed crystals and carrying out hydrothermal growth on the nickel film to obtain the nickel film-zinc oxide nanorod composite material.
Fig. 3 and 4 are a scanning electron micrograph and a transmission electron micrograph of the nickel film and zinc oxide nanorod composite material, respectively, and it can be seen that the rod-shaped zinc oxide grows on the surface of the nickel film.
Degradation of rhodamine B solution
The photocatalytic reaction is carried out in a series of XPA 7-type photocatalytic reactors produced by Nanjing Weijiang electromechanical plant, and the reaction temperature is 25 ℃. Putting the prepared nickel film and zinc oxide nanorod composite material into a quartz tube, adding 50mL of 10 mg/L rhodamine B solution, ultrasonically dispersing for 15min, and putting the mixture into a photocatalytic reactor. After dark reaction for 1 hour, an ultraviolet lamp is turned on to carry out photocatalytic degradation, 3ml of reaction liquid is taken every 10min, the reaction liquid is centrifuged for 5min by a centrifugal machine with the speed of 5000r/min, the supernatant liquid of the centrifugal tube is taken, and the absorbance of the supernatant liquid is detected by an ultraviolet spectrophotometer to obtain a photocatalytic degradation curve of the rhodamine B solution for reaction for 1 hour, which is shown in figure 5. As can be seen from fig. 5: the degradation rate of the composite material of the nickel film and the zinc oxide nano rod on rhodamine B reaches 85% when the reaction is carried out for 30min, and the degradation rate of the pure zinc oxide nano rod reaches 85% when the reaction is carried out for 50 min.
Degradation of ciprofloxacin solutions
The photocatalytic reaction is carried out in a series of XPA 7-type photocatalytic reactors produced by Nanjing Weijiang electromechanical plant, and the reaction temperature is 25 ℃. Putting the prepared nickel film and zinc oxide nanorod composite material into a quartz tube, adding 50mL of 10 mg/L ciprofloxacin solution, ultrasonically dispersing for 15min, and putting the composite material into a photocatalytic reactor. After the dark reaction is carried out for 1 hour, an ultraviolet lamp is turned on to carry out photocatalytic degradation, 3ml of reaction liquid is taken every 10min, the reaction liquid is centrifuged for 5min by a centrifugal machine with the speed of 5000r/min, the supernatant liquid of a centrifugal tube is taken, and an ultraviolet spectrophotometer is used for detecting the absorbance of the supernatant liquid, so that a photocatalytic degradation curve of the ciprofloxacin for reaction for 1 hour is obtained, and the graph is shown in FIG. 6. As can be seen in fig. 6: the degradation rate of the nickel film and zinc oxide nano-rod composite material to ciprofloxacin reaches 60% when the composite material reacts for 30min, the degradation rate reaches 87% in one hour, and the degradation rate of the pure zinc oxide nano-rod reaches 60% when the reaction lasts for about 45 min.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a nickel film and zinc oxide nanorod composite material is characterized by comprising the following steps:
(A) dropping collodion liquid into a clean and dry glass culture dish, rotating to uniformly disperse the collodion liquid, naturally drying the collodion liquid to obtain a collodion film, and taking off the collodion film for later use;
(B) injecting NiCl into the culture dish2·6H2O aqueous solution, sealed with the collodion film prepared in step (A), then inverted and inserted perpendicularly into the container containing KBH4After reacting for 24 hours at room temperature in a culture dish containing the solution, the solution is filled with NiCl2·6H2A black product is generated on one side of the collodion film of the O aqueous solution; collecting the black product, centrifuging and washing for several times, and vacuum drying at 60 ℃ to obtain a nickel film;
(C) dissolving anhydrous zinc acetate in absolute ethyl alcohol, pouring into a three-neck flask, and stirring in a constant-temperature oil bath at 60 ℃ until the zinc acetate is completely dissolved; dissolving potassium hydroxide in absolute ethyl alcohol for later use; slowly dripping a potassium hydroxide solution into a zinc acetate solution under the stirring condition of a constant-temperature oil bath at 60 ℃, and heating for 2 hours under the magnetic stirring condition to obtain ZnO seed crystals;
(D) taking a nickel film, dispersing the nickel film in PVP solution at room temperature, magnetically stirring for 4 hours, carrying out centrifugal separation, washing the obtained solid with absolute ethyl alcohol once, and removing redundant PVP molecules; dispersing the nickel film treated by PVP into the ZnO seed crystal solution prepared in the step (C), stirring for 3h, performing centrifugal separation, washing the solid product once by using ethanol, and attaching the nickel film with ZnO seed crystals;
(E) and then dispersing the nickel film attached with the ZnO seed crystal into an aqueous solution of zinc nitrate and hexamethylenetetramine with equal molar concentration, carrying out ultrasonic dispersion, reacting for 4 hours at 90 ℃, carrying out centrifugal separation on the product, washing twice with water and ethanol respectively, and carrying out vacuum drying at 60 ℃ to obtain the nickel film and zinc oxide nanorod nanocomposite.
2. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 1, characterized in that: the dropping amount of the collodion liquid in the step (A) is 7 mL.
3. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 1, characterized in that: NiCl adopted in step (B)2·6H2The concentration of the O aqueous solution was 5mmol/L, and the volume was 20 mL.
4. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 1, characterized in that: KBH used in step (B)4The concentration of the solution was 50mmol/L and the volume was 20 mL.
5. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 1, characterized in that: the zinc acetate solution in step (C) was prepared by weighing 0.2294g of anhydrous zinc acetate and dissolving in 125mL of anhydrous ethanol.
6. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 1, characterized in that: the potassium hydroxide solution in the step (C) was prepared by weighing 0.1094g of potassium hydroxide and dissolving in 65mL of absolute ethanol.
7. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 1, characterized in that: in step (D), 3mg of nickel film was weighed and dispersed in 20mL of 0.5g/L PVP solution.
8. The method for preparing the nickel film and zinc oxide nanorod composite material according to claim 7, characterized in that: and (E) dispersing the nickel film attached with the ZnO seed crystal into 20mL of zinc nitrate and hexamethylenetetramine aqueous solution with equal molar concentration, wherein the molar concentration of the zinc nitrate and the hexamethylenetetramine is 0.004M.
9. A nickel film and zinc oxide nanorod composite material obtained by the preparation method according to any one of claims 1 to 8.
10. The use of the nickel film and zinc oxide nanorod composite material of claim 9 in degradation of rhodamine B or ciprofloxacin.
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| "Nanostructures of Ni and NiCo amorphous alloys synthesized by a double composite template approach";Wen Ming et al;《JOURNAL OF PHYSICAL CHEMISTRY C》;20090324;第113卷(第15期);第5961页第2.2节，图1 * |
| "synthesis, characterization and photocatalytic activity of magnetically separable hexagonal Ni/ZnO nanostructure";Senapati samarpita et al;《NANOSCALE》;20120829;第4卷(第20期);第6605页左栏第2段以及第2.2节 * |
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