CN112875683A - Preparation method of graphene iron cyanide nickel cobalt nanocomposite - Google Patents

Preparation method of graphene iron cyanide nickel cobalt nanocomposite Download PDF

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CN112875683A
CN112875683A CN202110087821.3A CN202110087821A CN112875683A CN 112875683 A CN112875683 A CN 112875683A CN 202110087821 A CN202110087821 A CN 202110087821A CN 112875683 A CN112875683 A CN 112875683A
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郑国英
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Abstract

The invention discloses a preparation method of a graphene nickel cobalt ferricyanide nanocomposite, wherein a reverse micro-emulsion method is utilized to successfully synthesize a rGO/Ni-CoHCF nanocomposite, and Ni-CoHCF nanoparticles are uniformly attached to the surface of rGO, so that the rGO/Ni-CoHCF has a larger surface area, good wettability and excellent conductivity. These properties allow the rGO/Ni-CoHCF to have sufficient space for storing charge and transporting ions and electrons. Electrochemical tests are carried out by taking the rGO/Ni-COHCF nano composite material as a super capacitor electrode material, and the rGO/Ni-COHCF nano composite material is found to be used as a sodium ion battery anode material, so that the excellent electrochemical performance is also shown, and the application prospect is good.

Description

Preparation method of graphene iron cyanide nickel cobalt nanocomposite
Technical Field
The invention relates to the technical field of electrode material preparation, in particular to a preparation method of a graphene nickel cobalt ferricyanide nano composite material.
Background
Prussian-like blue is a class of artificially synthesized polymers with a framework structure. The Prussian-like blue material has the advantages of excellent electrochemical performance, easy synthesis, low price, no toxicity and the like, and is applied to the fields of energy storage, catalysis and sensors. Although the framework structure of the prussian blue can accommodate the intercalation and deintercalation of ions, the cyclic stability of the prussian blue is low due to poor conductivity. For this reason, modification thereof by means of doping or the like has attracted some researchers' attention. Compared with metal ions and metal oxides, the graphene has the characteristics of large specific surface area, excellent conductivity, high stability and the like, so that the graphene is considered to be an ideal dopant. In conclusion, doping is an effective means for improving the electrochemical performance of the prussian-like blue. However, uneven size, low yield and poor stability are still important factors for restricting the development and application of the prussian-like blue electrode material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a graphene nickel cobalt ferricyanide nanocomposite, which solves the problem that a new electrode material with uniform size, high yield and stability is formed by doping metal oxide with graphene.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a graphene nickel cobalt ferricyanide nanocomposite specifically comprises the following steps:
s1, under the ice-bath condition, mixing graphite and NaNO3、KMnO4Fully dissolved in a certain amount of concentrated H2SO4In (1). After the mixture was fully dissolved, the mixture was incubated at 35 ℃ for 45 min. Sequentially and slowly adding deionized water and H with a certain concentration2O2. Finally, washing the graphene oxide solution for multiple times by using a proper amount of diluted HCl and deionized water to obtain a graphene oxide solution;
s2, mixing a proper amount of the graphene oxide aqueous solution prepared in the step S1 and hydrazine hydrate with the same mass as the graphene oxide aqueous solution, and then carrying out certain treatment to obtain a reduced graphene (rGO) solution;
s3, then, taking C4H6NiO4·4H2O and C4H6CoO4·4H2Adding O into a certain amount of the reduced graphene (rGO) aqueous solution prepared in the step S2, and fully stirring to obtain a precursor solution;
s4, preparing two parts of a mixed solution of n-butyl alcohol, isooctane and hexadecyl trimethyl ammonium bromide, wherein the three substances are marked as a solution I and a solution II according to a certain mass ratio;
s5, mixing Ni contained in S32+And Co2+Is added to the solution one in the step S4. Will K3[Fe(CN)6]And adding the mixture into the second solution in the step S4. And then quickly mixing the two obtained mixed solutions, stirring, standing for 40h, fully cleaning with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 60 ℃ for 12h to obtain the graphene-nickel cobalt ferricyanide nano composite (rGO/Ni-CoHCF).
Preferably, H in step S12O2The concentration of (2) is 30%.
Preferably, the certain treatment in step S2 is heating to 98 ℃, and keeping the temperature for 24 h.
Preferably, the mass ratio of the n-butanol to the isooctane to the cetyltrimethylammonium bromide in the step S4 is 1:2: 1.
Advantageous effects
The invention provides a preparation method of a graphene nickel cobalt ferricyanide nanocomposite. Compared with the prior art, the method has the following beneficial effects: according to the preparation method of the graphene nickel cobalt ferricyanide nanocomposite, the rGO/Ni-CoHCF nanocomposite is successfully synthesized by using a reverse microemulsion method, and Ni-CoHCF nanoparticles are uniformly attached to the surface of rGO, so that the rGO/Ni-CoHCF has a larger surface area, good wettability and excellent conductivity. These properties allow the rGO/Ni-CoHCF to have sufficient space for storing charge and transporting ions and electrons. Electrochemical tests are carried out by taking the rGO/Ni-COHCF nano composite material as a super capacitor electrode material, and the rGO/Ni-COHCF nano composite material is found to be used as a sodium ion battery anode material, so that the excellent electrochemical performance is also shown, and the application prospect is good. The good electrochemical performance of the composite material is derived from the introduction of a two-dimensional layered graphene material, the agglomeration of Ni-CoHCF particles is effectively inhibited, the effective active sites of the Ni-CoHCF particles are increased, the electrochemical impedance of the Ni-CoHCF particles is reduced, and the electrochemical performance of the composite material is further improved.
Drawings
FIG. 1 is a flow diagram of the preparation of rGO/Ni-CoHCF nanocomposites of the present invention;
FIG. 2 is an FE-SEM photograph and TEM image of rGO/Ni-CoHCF (e, f) of the present invention (a), (b), (c), (d);
FIG. 3 is an electrochemical impedance spectrum of rGO/Ni-CoHCF and Ni-CoHCF of the present invention;
FIG. 4 is an XRD pattern of Ni-CoHCF and rGO/Ni-CoHCF of the present invention;
FIG. 5 is an infrared analysis of Ni-CoHCF and rGO/Ni-CoHCF of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-5, the embodiment of the present invention provides three technical solutions: a preparation method of a graphene nickel cobalt ferricyanide nanocomposite specifically comprises the following embodiments:
example 1
S1, under the ice-bath condition, 1.5g of graphite and 0.5g of NaNO are mixed3、3gKMnO4Fully dissolved in 36ml of concentrated H2SO4In (1). After the mixture was fully dissolved, the mixture was incubated at 35 ℃ for 45 min. 100ml of deionized water and 10ml of 30% H were added slowly in this order2O2. Finally, washing the graphene oxide solution for multiple times by using a proper amount of diluted HCl and deionized water to obtain a graphene oxide solution;
s2, mixing a proper amount of the graphene oxide aqueous solution prepared in the step S1 and hydrazine hydrate with the same mass as the graphene oxide aqueous solution, heating to 98 ℃, and preserving heat for 24 hours to obtain a reduced graphene (rGO) solution;
s3, then, taking 0.15mmolC4H6NiO4·4H2O and 0.15 mmoleC4H6CoO4·4H2Adding O into the reduced graphene (rGO) aqueous solution prepared in the step of 9mlS2, and fully stirring to obtain a precursor solution;
s4, preparing two parts of a mixed solution of n-butyl alcohol, isooctane and hexadecyl trimethyl ammonium bromide, wherein the three substances are marked as a solution I and a solution II according to a certain mass ratio;
s5, mixing Ni contained in S32+And Co2+Is added to the solution one in the step S4. Adding 0.5mmol L-1K3[Fe(CN)6]And adding the mixture into the second solution in the step S4. And then quickly mixing the two obtained mixed solutions, stirring, standing for 40h, fully cleaning with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 60 ℃ for 12h to obtain the graphene-nickel cobalt ferricyanide nano composite (rGO/Ni-CoHCF).
Example 2
S1, under the ice-bath condition, 4g of graphite and 1.2g of NaNO are mixed3、5gKMnO4Fully dissolved in 80ml of concentrated H2SO4In (1). After the mixture was fully dissolved, the mixture was incubated at 35 ℃ for 45 min. 220ml of deionized water and 22ml of 30% H were added slowly in this order2O2. Finally, washing the graphene oxide solution for multiple times by using a proper amount of diluted HCl and deionized water to obtain a graphene oxide solution;
s2, mixing a proper amount of the graphene oxide aqueous solution prepared in the step S1 and hydrazine hydrate with the same mass as the graphene oxide aqueous solution, heating to 98 ℃, and preserving heat for 24 hours to obtain a reduced graphene (rGO) solution;
s3, then, taking 0.32mmolC4H6NiO4·4H2O and 0.32 mmoleC4H6CoO4·4H2Adding O into the reduced graphene (rGO) aqueous solution prepared in the step of 20ml S2, and fully stirring to obtain a precursor solution;
s4, preparing two parts of a mixed solution of n-butyl alcohol, isooctane and hexadecyl trimethyl ammonium bromide, wherein the three substances are marked as a solution I and a solution II according to a certain mass ratio;
s5, mixing Ni contained in S32+And Co2+Is added to the solution one in the step S4. Adding 0.5mmol L-1K3[Fe(CN)6]And adding the mixture into the second solution in the step S4. And then quickly mixing the two obtained mixed solutions, stirring, standing for 40h, fully cleaning with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 60 ℃ for 12h to obtain the graphene-nickel cobalt ferricyanide nano composite (rGO/Ni-CoHCF).
Example 3
S1, under the ice-bath condition, 5g of graphite and 2g of NaNO are mixed3、7gKMnO4Fully dissolved in 100ml of concentrated H2SO4In (1). After the mixture was fully dissolved, the mixture was incubated at 35 ℃ for 45 min. 240ml of deionized water and 16ml of 30% H were added slowly in this order2O2. Finally, washing the graphene oxide solution for multiple times by using a proper amount of diluted HCl and deionized water to obtain a graphene oxide solution;
s2, mixing a proper amount of the graphene oxide aqueous solution prepared in the step S1 and hydrazine hydrate with the same mass as the graphene oxide aqueous solution, heating to 98 ℃, and preserving heat for 24 hours to obtain a reduced graphene (rGO) solution;
s3, then, taking 0.4mmolC4H6NiO4·4H2O and 0.4mmolC4H6CoO4·4H2Adding O into the reduced graphene (rGO) aqueous solution prepared in the step of 30mlS2, and fully stirring to obtain a precursor solution;
s4, preparing two parts of a mixed solution of n-butyl alcohol, isooctane and hexadecyl trimethyl ammonium bromide, wherein the three substances are marked as a solution I and a solution II according to a certain mass ratio;
s5, mixing Ni contained in S32+And Co2+Is added to the solution one in the step S4. Adding 0.5mmol L-1K3[Fe(CN)6]And adding the mixture into the second solution in the step S4. And then quickly mixing the two obtained mixed solutions, stirring, standing for 40h, fully cleaning with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 60 ℃ for 12h to obtain the graphene-nickel cobalt ferricyanide nano composite (rGO/Ni-CoHCF).
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. A preparation method of a graphene nickel cobalt ferricyanide nanocomposite is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, under the ice-bath condition, mixing graphite and NaNO3、KMnO4Fully dissolved in a certain amount of concentrated H2SO4In (1). After the mixture was fully dissolved, the mixture was incubated at 35 ℃ for 45 min. Sequentially and slowly adding deionized water and H with a certain concentration2O2. Finally, washing the graphene oxide solution for multiple times by using a proper amount of diluted HCl and deionized water to obtain a graphene oxide solution;
s2, mixing a proper amount of the graphene oxide aqueous solution prepared in the step S1 and hydrazine hydrate with the same mass as the graphene oxide aqueous solution, and then carrying out certain treatment to obtain a reduced graphene (rGO) solution;
s3, then, taking C4H6NiO4·4H2O and C4H6CoO4·4H2Adding O into a certain amount of the reduced graphene (rGO) aqueous solution prepared in the step S2, and fully stirring to obtain a precursor solution;
s4, preparing two parts of a mixed solution of n-butyl alcohol, isooctane and hexadecyl trimethyl ammonium bromide, wherein the three substances are marked as a solution I and a solution II according to a certain mass ratio;
s5, mixing Ni contained in S32+And Co2+Is added to the solution one in the step S4. Will K3[Fe(CN)6]And adding the mixture into the second solution in the step S4. And then quickly mixing the two obtained mixed solutions, stirring, standing for 40h, fully cleaning with deionized water and absolute ethyl alcohol, and then carrying out vacuum drying at 60 ℃ for 12h to obtain the graphene-nickel cobalt ferricyanide nano composite (rGO/Ni-CoHCF).
2. The method for preparing the graphene nickel cobalt ferricyanide nanocomposite according to claim 1, wherein the method comprises the following steps: h in the step S12O2The concentration of (2) is 30%.
3. The method for preparing the graphene nickel cobalt ferricyanide nanocomposite according to claim 1, wherein the method comprises the following steps: the certain treatment in the step S2 is heating to 98 ℃, and keeping the temperature for 24 h.
4. The method for preparing the graphene nickel cobalt ferricyanide nanocomposite according to claim 1, wherein the method comprises the following steps: the mass ratio of the n-butanol to the isooctane to the hexadecyl trimethyl ammonium bromide in the step S4 is 1:2: 1.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114032067A (en) * 2021-12-03 2022-02-11 中国海洋大学 CoFe @ C/rGO electromagnetic wave absorption composite material and preparation method thereof
CN114275799A (en) * 2022-03-04 2022-04-05 中博龙辉装备集团股份有限公司 Flexible self-supporting graphene/manganese hexacyanoferrate composite material and preparation method and application thereof
CN115240991A (en) * 2022-07-13 2022-10-25 辽宁大学 Construction method of novel ionic super capacitor based on electroactive ionic liquid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
邱小明: "碳基纳米复合材料的制备及其电化学性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114032067A (en) * 2021-12-03 2022-02-11 中国海洋大学 CoFe @ C/rGO electromagnetic wave absorption composite material and preparation method thereof
CN114032067B (en) * 2021-12-03 2023-08-01 中国海洋大学 CoFe@C/rGO electromagnetic wave absorption composite material and preparation method thereof
CN114275799A (en) * 2022-03-04 2022-04-05 中博龙辉装备集团股份有限公司 Flexible self-supporting graphene/manganese hexacyanoferrate composite material and preparation method and application thereof
CN114275799B (en) * 2022-03-04 2022-06-21 中博龙辉装备集团股份有限公司 Flexible self-supporting graphene/manganese hexacyanoferrate composite material and preparation method and application thereof
CN115240991A (en) * 2022-07-13 2022-10-25 辽宁大学 Construction method of novel ionic super capacitor based on electroactive ionic liquid
CN115240991B (en) * 2022-07-13 2023-09-15 辽宁大学 Manufacturing method of ionic supercapacitor based on electroactive ionic liquid

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