CN110241407B - Preparation method of large-area cobalt-nickel micro/nano periodic array structure film - Google Patents

Preparation method of large-area cobalt-nickel micro/nano periodic array structure film Download PDF

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CN110241407B
CN110241407B CN201910485490.1A CN201910485490A CN110241407B CN 110241407 B CN110241407 B CN 110241407B CN 201910485490 A CN201910485490 A CN 201910485490A CN 110241407 B CN110241407 B CN 110241407B
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cobalt
nickel
aqueous solution
nano
array structure
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CN110241407A (en
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翁凌燕
朱俐
陈忠平
龙朦朦
陆敏
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Nantong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/48—Coating with alloys
    • C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel

Abstract

The invention discloses a preparation method of a large-area cobalt-nickel micro/nano periodic array structure film, which comprises the steps of firstly respectively preparing a cobalt nitrate aqueous solution and a nickel nitrate aqueous solution, mixing the two solutions, adjusting the pH value to 4-5 to obtain a cobalt-nickel metal salt composite aqueous solution, slowly adding a urea aqueous solution, mixing to obtain a reaction solution, immersing a pretreated butterfly wing serving as a template into the reaction solution, carrying out closed heating reaction under the condition of an external magnetic field to obtain the butterfly wing with the cobalt-nickel micro/nano periodic array structure, washing the butterfly wing with deionized water, acetone and absolute ethyl alcohol in sequence, and drying. The invention takes the butterfly wing as a template, adopts urea as a precipitator, and grows the cobalt-nickel micro/nano periodic array structure material on the butterfly wing by a chemical method by a liquid phase method under the control of an external magnetic field, thereby having simple preparation process, low cost and high operability.

Description

Preparation method of large-area cobalt-nickel micro/nano periodic array structure film
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a large-area cobalt-nickel micro/nano periodic array structure film.
Background
The large-area periodic nano array structure is continuously concerned by basic subjects and application technologies such as optics, microfluidics, bionics, surface coatings, supercapacitors, antifogging, self-cleaning, biosensors and the like in recent years because the periodic nano array structure can provide a very high specific surface area, a very large number of ion transmission channels, good conductivity and capability of preventing curing and agglomeration. The micro/nano periodic array structure is a design better than a first-level nano array, the composite material with the nano multistage structure connects functional materials with different structures and different phase states in series, the characteristics of each part can be excited, a synergistic effect is formed, the electronic ion conductivity, the electrochemical reaction activity, the mechanical stability, the electrochemical reaction stability and the cycling stability of an electrode material can be improved even if the single-phase material with the nano multistage structure is adopted, and a perfect solution can be brought to quicker and larger energy storage by manufacturing the electrode on a large scale of a large-area micro/nano periodic array structure film.
Cobalt has wide application in the fields of magnetic materials, catalytic materials, gas sensors and the like, and in pure cobalt, an optical transition which has photon energy of about 4.5eV and contributes to magneto-optical rotation exists; as an important material of the battery anode, the metallic nickel has the characteristics of high specific volume, high specific power and the like, so that the cobalt nickel is widely applied to the fields of optics, magnetics and catalysis. The cobalt-nickel nano fiber material is a one-dimensional magnetic nano material, the magnetic property, the catalytic property, the microwave absorption property and the like of the cobalt-nickel nano fiber material are changed along with the difference of particle chemical composition and grain size, and the cobalt-nickel nano fiber material has wide application in the fields of microwave absorption, thermotherapy, catalysis, magnetic resonance imaging, drug delivery systems, magnetic recording, magnetic sensors and the like, so that the cobalt-nickel micro/nano periodic array structure material has wide development prospect and application space.
The current preparation methods of periodic nano array structure materials are 2 types, namely a template method and a laser etching method.
The template method is a preparation method capable of effectively controlling the granularity and the morphology of powder, various quasi-one-dimensional nano materials are prepared by selecting a specific sample mold and growing in a limited area, and a new material which cannot be prepared by a conventional system is obtained. The quasi-one-dimensional nano material prepared by the template method has various types, easily obtained raw materials, uniform powder appearance and small diameter distribution range, and the diameter and the length of the powder structure can be regulated and controlled by adjusting various parameters of the template or selecting different templates, thereby playing an important role in synthesizing the ordered nano quasi-one-dimensional nickel-cobalt alloy material. The technology is most typically characterized in that the size and the shape of the prepared one-dimensional material are controlled through the confinement capability provided by the template, and the nano material and the nano array with various required structures can be prepared. The template is a film which contains high-density nanometer column-shaped holes and has the thickness of dozens to hundreds of microns, and the template selected at present mainly comprises a porous anodic aluminum oxide film, track etching, a polymer film, a zeolite molecular sieve, a carbon nanometer tube and the like. The technology has the defects that a nano-scale template with excellent performance needs to be purchased or manufactured, the preparation process is complex, and the manufacturing cost of the periodic nano-array structure material is increased.
The laser etching method is to combine the laser surface processing technology and the nanotechnology to realize a surface layer with nanometer characteristics, which can be collectively called as a laser surface nanocrystallization technology, directly or mainly utilizes the specific technical means of laser to directly change or add materials to change the form, components or structure of the surface of a processed solid material so as to form a surface layer containing nanometer grains or certain nanometer particle components, and mainly adopts the means of laser etching, laser imprinting, laser texturing, laser micro-nano modeling and the like to realize the nanometer structure on the surface of the material. The most typical technique is laser surface nanoimprint, which can very precisely define the angle and vertical plane, and form large-area patterns on a metal sheet by using 3D structures in the nanometer scale. Although the laser surface nanocrystallization technology realizes the leap-type progress in preparing the nano surface structure material, the problems of complex preparation process, high price, low operation freedom degree and the like are not negligible.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a preparation method of a large-area cobalt-nickel micro/nano periodic array structure film, aiming at the defects of the prior art, and the method has the advantages of low cost, simple raw materials and convenient operation.
The technical scheme is as follows: a preparation method of a large-area cobalt-nickel micro/nano periodic array structure film comprises the following steps:
step 1, respectively preparing a cobalt nitrate aqueous solution and a nickel nitrate aqueous solution, mixing the two solutions, adjusting the pH value to 4-5 to obtain a cobalt-nickel metal salt composite aqueous solution, wherein the stoichiometric ratio of Co/Ni is 1: 1-8: 1, adding a urea aqueous solution, and mixing to obtain a reaction solution;
step 2, immersing the pretreated butterfly wing serving as a template into the reaction solution in the step 1, and carrying out closed heating reaction under the condition of an external magnetic field to obtain the butterfly wing with the cobalt-nickel micro/nano periodic array structure;
and 3, taking out the butterfly wing, washing the butterfly wing with deionized water, acetone and absolute ethyl alcohol in sequence, and drying the butterfly wing.
Further, in the step 1, the concentration of the cobalt nitrate aqueous solution is 0.01-0.5 mol/L, the concentration of the nickel nitrate aqueous solution is 0.01-0.5 mol/L, the concentration of the urea aqueous solution is 0.03-1.00 mol/L, and 300-600 mL of urea solution is added per 100mL of the cobalt-nickel metal salt composite aqueous solution.
Further, the pretreatment process of the butterfly wings in the step 2 is as follows: treating butterfly wings with 1mM HCl solution at 50 deg.C for 3 hr, treating butterfly wings with 2mM NaOH solution at 60 deg.C for 6 hr, and washing butterfly wings with double distilled water to remove excessive NaOH.
Further, the strength of the external magnetic field in the step 2 is 0.01-1.00T, and the heating reaction condition is that the temperature is heated to 60-100 ℃ in a water bath.
Further, the drying conditions in the step 3 are 40-80 ℃ and 1-2 h.
Has the advantages that: the invention takes the butterfly wing as a template, adopts urea as a precipitator, and grows large-area cobalt-nickel micro/nano periodic array structure materials on the butterfly wing by a liquid phase method by a chemical method under the control of an external magnetic field with the strength of 0.01T-1.00T, and the preparation process is simple, the cost is low, and the operability is high.
The invention adopts a cobalt-nickel metal salt composite aqueous solution precipitation system, firstly takes butterfly wings as effective templates, and controls the shape of cobalt and nickel structure crystal ions after coprecipitation on the surfaces of the cobalt and nickel structure crystal ions through the action of an external magnetic field with the strength of 0.01T-1.00T, thereby preparing the large-area cobalt-nickel micro/nano periodic array structure film material. The cobalt-nickel precursor precipitates are easy to form microspheres, but the order and periodicity of the precipitate morphology are controlled due to the existence of a submicron structure on the butterfly wing, so that a periodically repeated chrysanthemum-shaped micro/nano cobalt-nickel material can be formed on the surface of the butterfly wing; under the action of an external magnetic field of 0.01T-1.00T, cobalt and nickel crystal-forming ions in a reaction system are deposited on the surface of the submicron structure uniformly, so that accumulation can be avoided. The cobalt-nickel metal salt composite aqueous solution precipitation system takes butterfly wings as templates, periodically and orderly grows on the surfaces of the submicron structures of the butterfly wings, is orderly arranged and uniformly covered, so that a large-area cobalt-nickel micro/nano periodic array structure film is formed, the problems of complex preparation process, high cost, low operable degree of freedom and the like in the traditional micro-nano structure preparation process are solved, and further popularization and application of the cobalt-nickel micro/nano periodic array structure film are facilitated.
The method adopts a chemical solution method for reaction, has simple conditions, convenient operation, low cost of raw materials and environmental protection, and provides conditions for the practical application of the cobalt-nickel micro/nano periodic array structure film.
Drawings
FIG. 1 is a FESEM photograph of a cobalt nickel nanofiber film prepared in example 1, with a 10 μm scale.
FIG. 2 is a FESEM photograph of a cobalt nickel nanofiber film prepared in example 1, with a 1 μm scale.
FIG. 3 is a FESEM photograph of a cobalt nickel nanofiber film prepared in example 2, with a 20 μm scale.
FIG. 4 is a FESEM photograph of a cobalt nickel nanofiber film prepared in example 2, with a 1 μm scale.
FIG. 5 is a FESEM photograph of a cobalt nickel nanofiber film prepared in example 3, with a scale of 100 μm.
FIG. 6 is a FESEM photograph of a cobalt nickel nanofiber film prepared in example 3, with a 2 μm scale.
Detailed Description
The technical solution of the present invention is further explained below with reference to the specific embodiments and the accompanying drawings.
Example 1
First step, preparation of reaction solution: 2.3925g of cobalt nitrate hexahydrate Co (NO) was accurately weighed3)2·6H2O and 0.727g of Ni nitrate hexahydrate (NO)3)2·6H2And placing O in a beaker, respectively adding 100mL of deionized water, mixing after dissolving, stirring for 2 hours at room temperature to fully dissolve metal soluble salt in the deionized water, and then adding 2mol/L of HCL solution to adjust the pH value to 4 to obtain the cobalt-nickel metal salt composite aqueous solution. In addition, 12g of urea is accurately weighed and placed in a beaker, 600mL of deionized water is added, and the mixture is fully stirred to be dissolved, so that urea solution is obtained. Under the condition of magnetic stirring, slowly adding the prepared urea solution into the cobalt-nickel metal salt composite solution to obtain a reaction solution, and standing for later use.
Secondly, preparing the cobalt-nickel micro/nano periodic array structure film: the butterfly wings were treated with 1mM HCl solution at 50 ℃ for 3 h, followed by 2mM NaOH solution at 60 ℃ for 6 h, after which the butterfly wings were rinsed with double distilled water to remove excess NaOH. After the pretreatment, the butterfly wing is immersed into the cobalt-nickel metal salt mixed solution added with the precipitator, and the reaction vessel is sealed after the butterfly wing sinks into the bottom of the reaction vessel.
Thirdly, preparing the cobalt-nickel micro/nano periodic array structure film: and (3) putting the sealed reaction container into a water bath, heating to 90 ℃, and simultaneously applying an external magnetic field of 0.05T to react for 42 hours until the reaction is finished. Taking out the butterfly wing with the cobalt-nickel micro/nano periodic array structure film from the reaction container, washing the butterfly wing with deionized water, acetone and absolute ethyl alcohol for 2 to 3 times in sequence, and then placing the butterfly wing in an oven to dry for 5 hours at low temperature.
The FESEM photographs of the cobalt-nickel micro/nano periodic array structure thin film prepared in this example are shown in fig. 1 and 2.
And (4) conclusion: FESEM test shows that the prepared cobalt-nickel nano material is regularly and closely arranged on the submicron structure surface of the butterfly wing in a gold-wire chrysanthemum-shaped periodic manner in a large area. Each chrysanthemum is about 2-2.5 μm in size, the flowers are tiled and arranged, the nano gaps are formed in a staggered and ordered mode, the size range of the gaps is 200-500 nm, the nano wires exactly like the chrysanthemum filaments are uniformly radiated from the points to the periphery, and the diameter of the nano wires is about 20-50 nm. Scanning electron micrographs show that the series of products have a golden-silk chrysanthemum-shaped micro/nano periodic ordered arrangement structure on the surface of butterfly wings, and the cobalt-nickel micro/nano periodic array structure film with a uniform surface structure is prepared.
Example 2
This example differs from example 1 in that: no external magnetic field of 0.05T is applied during the preparation process of the third step.
First step, preparation of reaction solution: 2.3925g of cobalt nitrate hexahydrate Co (NO) was accurately weighed3)2·6H2O and 0.727g of Ni nitrate hexahydrate (NO)3)2·6H2Placing O in a beaker, respectively adding 100mL of deionized water, dissolving, mixing, and stirring at room temperature for 2 hours to allow gold to be attachedAnd fully dissolving soluble salt in deionized water, and then adding 2mol/L HCL solution to adjust the pH value to 4 to obtain the cobalt-nickel metal salt composite aqueous solution. In addition, 12g of urea is accurately weighed and placed in a beaker, 600mL of deionized water is added, and the mixture is fully stirred to be dissolved, so that urea solution is obtained. Under the condition of magnetic stirring, slowly adding the prepared urea solution into the cobalt-nickel metal salt composite solution to obtain a reaction solution, and standing for later use.
Secondly, preparing the cobalt-nickel micro/nano periodic array structure film: the butterfly wings were treated with 1mM HCl solution at 50 ℃ for 3 h, followed by 2mM NaOH solution at 60 ℃ for 6 h, after which the butterfly wings were rinsed with double distilled water to remove excess NaOH. After the pretreatment, the butterfly wing is immersed into the cobalt-nickel metal salt mixed solution added with the precipitator, and the reaction vessel is sealed after the butterfly wing sinks into the bottom of the reaction vessel.
Thirdly, preparing the cobalt-nickel micro/nano periodic array structure film: and putting the sealed reaction container into a water bath, heating to 90 ℃, and reacting for 42 hours until the reaction is finished. Taking out the butterfly wing with the cobalt-nickel micro/nano periodic array structure film from the reaction container, washing the butterfly wing with deionized water, acetone and absolute ethyl alcohol for 2 to 3 times in sequence, and then placing the butterfly wing in an oven to dry for 5 hours at low temperature.
FESEM pictures of the cobalt-nickel micro/nano periodic array structure thin film prepared in this example are shown in FIGS. 3 and 4. As can be seen from fig. 3 and 4, although the prepared cobalt-nickel micro/nano periodic array structure thin film has a large area and is partially arranged in a golden daisy shape, the periodic regularity is weak, and the sea urchins are staggered and overlapped in multiple layers.
Example 3
This example differs from example 1 in that: in the preparation process of the second step, nano paper with the aperture of 7-10 mu m is used as an effective template.
First step, preparation of reaction solution: 1.485g of cobalt nitrate hexahydrate Co (NO) was accurately weighed3)2·6H2O and 0.727g of Ni nitrate hexahydrate (NO)3)2·6H2Placing O in a beaker, adding 100mL of deionized water respectively, and dissolvingAnd mixing after decomposition, stirring for 3 hours at room temperature to fully dissolve metal soluble salt in deionized water, and then adding 0.2mol/L HCL solution to adjust the pH value to 5.5 to obtain the cobalt-nickel metal salt composite aqueous solution. In addition, 9g of urea is accurately weighed and placed in a beaker, 300mL of deionized water is added, and the mixture is fully stirred to be dissolved, so that a urea solution is obtained. Under the condition of magnetic stirring, slowly adding the prepared urea solution into the cobalt-nickel metal salt composite solution to obtain a reaction solution, and standing for later use.
Secondly, preparing the cobalt-nickel micro/nano periodic array structure film: and (3) washing the nano paper with the aperture of 7-10 microns for three times by using deionized water, then immersing the nano paper into the mixed solution of the cobalt and nickel metal salts added with the precipitator, and sealing the reaction vessel after the nano paper is immersed at the bottom of the reaction vessel.
Thirdly, preparing the cobalt-nickel micro/nano periodic array structure film: and (3) putting the sealed reaction container into a water bath, heating to 80 ℃, and simultaneously applying an external magnetic field of 0.05T to react for 48 hours until the reaction is finished. And taking out the butterfly nanopaper on which the cobalt-nickel micro/nano periodic array structure film grows from the reaction container, washing the butterfly nanopaper for 2 to 3 times by using deionized water, acetone and absolute ethyl alcohol in sequence, and then placing the butterfly nanopaper in an oven to dry the butterfly nanopaper for 3.5 hours at low temperature.
FESEM pictures of the cobalt nickel micro/nano thin film prepared in this example are shown in FIGS. 5 and 6.
As can be seen from FIGS. 5 and 6, the prepared cobalt-nickel micro/nano film is randomly arranged on the nano paper in a large area, and after the local area is enlarged, the micro fibers on the nano paper are closely stacked in a chrysanthemum shape, the periodicity is weak, and the flowers are overlapped.
In conclusion, the invention prepares the large-area cobalt-nickel micro/nano periodic array structure on the butterfly wing by a simple chemical method. The specific appearance of the cobalt-nickel micro/nano periodic array structure on the butterfly wing is controlled by the submicron structure on the surface of the butterfly wing, different types of butterfly wings can prepare micro/nano periodic array structures with different appearances, and the effect of an external magnetic field with the strength of 0.01T-1.00T is assisted to control the uniform deposition of cobalt and nickel crystal ions on the surface of the submicron structure so as to avoid the accumulation phenomenon. FESEM tests show that the cobalt-nickel micro/nano periodic array structure film prepared in example 1 has diversified surface morphologies on butterfly wings, a shape with golden chrysanthemum periodic ordered close arrangement and a shape with sea urchin periodic ordered close arrangement. The structure of the cobalt-nickel micro/nano periodic array ensures that the material has the characteristics of light weight and high strength, the nano fiber structure with a certain length-diameter ratio ensures that a macroscopic film has larger additional surface area, the electronic ion conductivity, the electrochemical reaction activity, the mechanical stability, the electrochemical reaction stability and the cycle stability of the material are improved, and meanwhile, the large-scale manufacturing of the electrode of the micro/nano periodic array structure film can bring a perfect solution for faster and larger energy storage.

Claims (3)

1. A preparation method of a large-area cobalt-nickel micro/nano periodic array structure film is characterized by comprising the following steps: the method comprises the following steps:
step 1, respectively preparing a cobalt nitrate aqueous solution and a nickel nitrate aqueous solution, mixing the two solutions, adjusting the pH value to 4-5 to obtain a cobalt-nickel metal salt composite aqueous solution, wherein the stoichiometric ratio of Co/Ni is 1: 1-8: 1, adding a urea aqueous solution, and mixing to obtain a reaction solution;
step 2, immersing the pretreated butterfly wing serving as a template into the reaction solution in the step 1, and carrying out closed heating reaction under the condition of an external magnetic field to obtain the butterfly wing with the cobalt-nickel micro/nano periodic array structure;
step 3, taking out the butterfly wing, washing the butterfly wing with deionized water, acetone and absolute ethyl alcohol in sequence, and drying the butterfly wing;
wherein:
the pretreatment process of the butterfly wings in the step 2 comprises the following steps: treating butterfly wings with 1mM HCl solution at 50 deg.C for 3 h, treating butterfly wings with 2mM NaOH solution at 60 deg.C for 6 h, and washing butterfly wings with double distilled water to remove excessive NaOH;
in the step 2, the strength of the external magnetic field is 0.01-1.00T, and the heating reaction condition is that the temperature is heated to 60-100 ℃ in a water bath.
2. The production method according to claim 1, characterized in that: in the step 1, the concentration of the cobalt nitrate aqueous solution is 0.01-0.5 mol/L, the concentration of the nickel nitrate aqueous solution is 0.01-0.5 mol/L, the concentration of the urea aqueous solution is 0.03-1.00 mol/L, and 300-600 mL of urea solution is added per 100mL of the cobalt-nickel metal salt composite aqueous solution.
3. The production method according to claim 1, characterized in that: the drying condition in the step 3 is 40-80 ℃ and 1-2 h.
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