CN110428976A - A kind of preparation method and applications of Cu-Co-S-MOF nanometer sheet - Google Patents

A kind of preparation method and applications of Cu-Co-S-MOF nanometer sheet Download PDF

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Publication number
CN110428976A
CN110428976A CN201910640910.9A CN201910640910A CN110428976A CN 110428976 A CN110428976 A CN 110428976A CN 201910640910 A CN201910640910 A CN 201910640910A CN 110428976 A CN110428976 A CN 110428976A
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China
Prior art keywords
mof
nanometer sheet
solution
cobalt
nitrate hexahydrate
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CN201910640910.9A
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Chinese (zh)
Inventor
蒋继波
孙瑶馨
陈宇凯
王露露
胡晓敏
丛海山
刘凤茹
高丽
常宾
康佳玲
唐佳斌
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上海应用技术大学
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Priority to CN201910640910.9A priority Critical patent/CN110428976A/en
Publication of CN110428976A publication Critical patent/CN110428976A/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features, e.g. forms, shapes, surface areas, porosities or dimensions, of the materials making up or comprised in the electrodes; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their materials
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The present invention relates to a kind of preparation methods of Cu-Co-S-MOF nanometer sheet, the following steps are included: S1: Cobalt(II) nitrate hexahydrate is dissolved in deionized water, obtain solution A, 2-methylimidazole is dissolved in deionized water, obtain solution B, clean nickel foam is added later and is reacted for mixed solution A and solution B, obtains the nickel foam with Co-MOF;S2: copper nitrate hexahydrate, Cobalt(II) nitrate hexahydrate being dissolved in isopropanol, mixed solution C is obtained after dissolution, and carbon disulfide and pentamethyl-diethylenetriamine are added into mixed solution C, obtains mixed solution D;S3: the nickel foam with Co-MOF is added in mixed solution D, and is transferred in reaction kettle and carries out hydro-thermal reaction, obtains Cu-Co-S-MOF nanometer sheet after reaction.Compared with prior art, preparation method of the present invention is environmental-friendly, preparation method process is simple, and convenient for large-scale production, the Cu-Co-S-MOF nanometer sheet of acquisition is applied to that more excellent chemical property can be obtained when electrode material.

Description

A kind of preparation method and applications of Cu-Co-S-MOF nanometer sheet

Technical field

The present invention relates to electrochemistry and technical field of nano material, more particularly, to a kind of Cu-Co-S-MOF nanometer sheet Preparation method and applications.

Background technique

The increasingly consumption and the discharge of greenhouse gases of fossil fuel generate very big influence to environment, cause the whole world right The demand of sustainable energy supply constantly increases.But only sustainable energy be it is inadequate, the world today more there is an urgent need to The energy storage device of one kind efficiently, stable, environmentally friendly is explored to improve energy storage efficiency.Supercapacitor (SC) is used as a kind of high power Density, long circulation life, energy storage device at low cost, the charge and discharge time is fast, have received widespread attention, so to renewable clear The exploitation of the clean energy, using becoming more and more important.

The electrode of conventional slurries paint-on technique preparation is there are two disadvantage: one side surface area is smaller, cause capacitive property by To limitation;It on the other hand is that used adhesive can reduce conductivity.

Metal organic framework is with its unique crystal structure and Chemical Diversity, in water-splitting, fuel cell, solar-electricity The application in the fields such as pond, lithium ion battery, stem cell, sensor and biosensor receives significant attention.Recently, many researchs All concentrate on designing and manufacturing for the MOFs with adjustable pattern.However, designing and manufacturing for MOFs is not a kind of practical Or cost-effective method, which prevent they commercial field practical application.In order to obtain bigger cost-effectiveness, It needs simplification and designs and manufactures the MOFs with high electrochemical performance.In recent years, has a small amount of MOFs as SCs electrode material The report of material, but their special capacity and rate capability are relatively low, and since preparation method is only applicable to laboratory mould Formula causes industrial applications that can not implement.

Summary of the invention

It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of Cu-Co-S-MOF The preparation method and applications of nanometer sheet.

A kind of preparation method of Cu-Co-S-MOF nanometer sheet, comprising the following steps:

S1: Cobalt(II) nitrate hexahydrate is dissolved in deionized water, obtains solution A, and 2-methylimidazole is dissolved in deionized water In, solution B, mixed solution A and solution B are obtained, stirs, clean nickel foam is added later and is reacted, after reaction will Reaction product drying, obtains the nickel foam with Co-MOF;

S2: copper nitrate hexahydrate, Cobalt(II) nitrate hexahydrate being dissolved in isopropanol, mixed solution C is obtained after dissolution, Carbon disulfide and pentamethyl-diethylenetriamine are added into mixed solution C, obtains mixed solution D;

S3: the nickel foam with Co-MOF being added in mixed solution D, and is transferred in reaction kettle and carries out hydro-thermal reaction, Cu-Co-S-MOF nanometer sheet is obtained after reaction.

Further, the Cu-Co-S-MOF nanometer sheet is with CuCo2S4The nickel foam of@Co-MOF.

Further, the organic backbone in the Cu-Co-S-MOF nanometer sheet is cobalt-based metal organic framework.

Further, Cobalt(II) nitrate hexahydrate and 2-methylimidazole molar ratio are 1:8 in step S1.

Further, copper nitrate hexahydrate and Cobalt(II) nitrate hexahydrate molar ratio are 1:2 in the mixed solution C.

Further, in step S3, carbon disulfide and pentamethyl-diethylenetriamine volume ratio are 1:8.3.

Further, it in step S3, obtains being immediately placed in reaction kettle after mixed solution D carrying out hydro-thermal reaction, reaction temperature Degree is 150 DEG C, reaction time 8h.

Cu-Co-S-MOF nanometer sheet prepared by the present invention can be applied widely in electrode material.

Transient metal sulfide has higher electric conductivity and better redox property than transition metal oxide, CuCo2S4Its theoretical specific capacity is high, at low cost, and cobalt and copper ion have stronger redox property, Ternary copper cobalt sulfide (CuCo2S4) chemical property be better than binary metal copper sulfide or cobalt sulfide.Further, since the electronegativity of sulphur is lower, CuCo2S4Compared with Cu, Co oxide, there is excellent electric conductivity, higher electro catalytic activity and higher theoretical capacity.This Invention is prepared for porous carbon/metal oxide by template of MOFs, and is applied to energy storage device, since MOFs is with higher Surface area and unique porosity, directly as electroactive material be applied to energy storage field, realize higher electrochemistry Can, the present invention enhances the chemical property of original MOFs using Cu, Co metal ion and ligand, so that chemical property is significant It improves.

The present invention compared with the existing technology, has the following advantages and beneficial effects:

1, the present invention directly synthesizes CuCo in nickel foam2S4@Co-MOF electrode material, greatly simplified reaction step, Improve preparation efficiency, solution produced during the preparation process is pollution-free, and whole preparation process atom utilization is high, prepare material at This is low, therefore can carry out large-scale industrial production.

2, CuCo prepared by the present invention2S4The most important characteristic of@Co-MOF first is that nano material be in 3 D stereo globular flower Clustering architecture (such as Fig. 1).

3, CuCo prepared by the present invention2S4@Co-MOF nanometer sheet has very high specific capacitance, up to 950F/g.

Detailed description of the invention

Fig. 1 is CuCo made from embodiment 12S4SEM figure of the@Co-MOF nano material under 1 μm;

Fig. 2 is CuCo made from embodiment 12S4SEM figure of the@Co-MOF nano material under 10 μm;

Fig. 3 is CuCo made from embodiment 12S4The CV of@Co-MOF nano material schemes;

Fig. 4 is CuCo made from embodiment 12S4The GCD of@Co-MOF nano material schemes.

Specific embodiment

The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.

Embodiment 1

Cobalt-based metal organic framework (Co-MOF): 0.05M is grown on nickel foam (1cm × 1cm) using solwution method first Cobalt(II) nitrate hexahydrate is dissolved in 40ml deionized water, is called solution A.0.4M 2-methylimidazole is dissolved in 40ml deionized water In, it is called solution B.Solution A is mixed rapidly with solution B, is then placed in clean nickel foam and reacts 4h under room temperature. To after reaction, the nickel foam for having Co-MOF is rinsed with ethyl alcohol and deionized water, and is placed it in 60 DEG C of drying box It is dried.

Secondly 0.5mmol copper nitrate hexahydrate, 1mmol Cobalt(II) nitrate hexahydrate are dissolved in 5ml isopropanol, to it Mixed solution C is obtained after being completely dissolved, and adds 120 μ l carbon disulfide and 1ml pentamethyl-diethylenetriamine (PMDTA) is mixed Solution D, and the nickel foam with Co-MOF is immersed in mixed solution D, then it is quickly transferred to polytetrafluoroethylene (PTFE) hydro-thermal 150 DEG C of solvent thermal reaction are carried out in kettle, 8h.After reacting end and being cooled to room temperature, CuCo will be had2S4The nickel foam of@Co-MOF It takes out, is successively cleaned 3 times with deionized water and ethyl alcohol, be then placed in vacuum oven 60 DEG C, 12h.

The method for using cyclic voltammetry and constant current charge-discharge through occasion China CHI760e electrochemical workstation, detects the material Specific capacitance and stable circulation performance, cyclic voltammetry test, it is shown that material has excellent redox ability.It utilizes Electronic scanner microscope (surface microstructure for characterizing the electrode material), the high-specific surface area for super electric material provides base Plinth.In 2M KOH solution and under the current density of 1A/g, the specific capacitance of electrode material of the present invention has reached 950F/g.Such as figure 1 Fig. 2 shows that the pattern of the electrode material is that cluster is spherical, increases the specific surface area of three-dimensional structure, can sufficiently connect with electrolyte Touching, ion exchange are more quick.Specific capacitance can be calculated in 1Ag according to Fig. 4 GCD curve-1Current density under, specific capacitance 950F/g can be reached.

Embodiment 2

Clean nickel foam is got out for (what is selected here be clean nickel foam to be substrate, real in following experiment Apply example 1 need to be with the nickel foam of Co-MOF be substrate).By 0.5mmol copper nitrate hexahydrate, 1mmol cobalt nitrate six Hydrate dissolution is in 5ml isopropanol, after it is completely dissolved, adds 120 μ l carbon disulfide and 1ml pentamethyl-diethylenetriamine (PMDTA), it and by the submergence of clean nickel foam in the solution, is then quickly transferred in polytetrafluoroethylene (PTFE) water heating kettle and is carried out 150 DEG C of solvent thermal reaction, 8h.After reacting end and being cooled to room temperature, CuCo will be had2S4Nickel foam take out, use deionized water It is successively cleaned with ethyl alcohol 3 times, is then placed in vacuum oven 60 DEG C, 12h.

The method for using cyclic voltammetry and constant current charge-discharge through occasion China CHI760e electrochemical workstation, detects the material Specific capacitance and cyclical stability performance, cyclic voltammetry test, it is shown that material has excellent redox ability.Benefit With electronic scanner microscope (surface microstructure for characterizing the electrode material), the high-specific surface area for super electric material provides base Plinth.In 2M KOH solution and under the current density of 0.5A/g, the specific capacitance of electrode material of the present invention has reached 520F/g.

Comparative example 1

The form of the copper cobalt sulfide electrode material of the other patterns synthesized in the present embodiment, synthetic material and specific capacitance ginseng Be shown in Table 1, by the structure that is synthesized in the visible embodiment 1 of result under identical test environment specific capacitance value with higher.

The form of 1. bronze medal cobalt sulfide electrode material of table, synthetic material and specific capacitance

Bibliography in table 1:

[1]Guo S H,Chen W Q,Li M,et al.Effect of reaction temperature on the amorphous-crystalline transition of copper cobalt sulfide for supercapacitors [J]. Electrochimica Acta,2018,271,498-506.

[2]Lee Y H,Kang B K,Kim M S,et al.Synthesis and Characterization of Highly Uniform CuCo2S4Ball-in-Ball Hollow Nanospheres as High Performance Electrode for Supercapacitors[J].physica status solidi(a),2018,215(20): 1700936.

[3]Wang T,Liu M,Ma H.Facile synthesis of flower-like copper-cobalt sulfide as binder-free faradaic electrodes for supercapacitors with improved electrochemical properties[J].Nanomaterials,2017,7(6):140.

[4]Jin C,Cui Y,Zhang G,et al.Synthesis of copper-cobalt hybrid oxide microflowers as electrode material for supercapacitors[J].Chemical Engineering Journal,2018,343: 331-339.

The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention. Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention Within protection scope.

Claims (8)

1. a kind of preparation method of Cu-Co-S-MOF nanometer sheet, which comprises the following steps:
S1: Cobalt(II) nitrate hexahydrate is dissolved in deionized water, obtains solution A, and 2-methylimidazole is dissolved in deionized water, is obtained To solution B, clean nickel foam is added later and is reacted for mixed solution A and solution B, stirring, after reaction produces reaction Object drying, obtains the nickel foam with Co-MOF;
S2: copper nitrate hexahydrate, Cobalt(II) nitrate hexahydrate being dissolved in isopropanol, mixed solution C is obtained after dissolution, to mixed It closes and carbon disulfide and pentamethyl-diethylenetriamine is added in solution C, obtain mixed solution D;
S3: the nickel foam with Co-MOF being added in mixed solution D, and is transferred in reaction kettle and carries out hydro-thermal reaction, is reacted After obtain Cu-Co-S-MOF nanometer sheet.
2. a kind of preparation method of Cu-Co-S-MOF nanometer sheet according to claim 1, which is characterized in that the Cu- Co-S-MOF nanometer sheet is with CuCo2S4The nickel foam of@Co-MOF.
3. a kind of preparation method of Cu-Co-S-MOF nanometer sheet according to claim 2, which is characterized in that the Cu- Organic backbone in Co-S-MOF nanometer sheet is cobalt-based metal organic framework.
4. a kind of preparation method of Cu-Co-S-MOF nanometer sheet according to claim 1, which is characterized in that in step S1 Cobalt(II) nitrate hexahydrate and 2-methylimidazole molar ratio are 1:8.
5. a kind of preparation method of Cu-Co-S-MOF nanometer sheet according to claim 1, which is characterized in that described is mixed Closing copper nitrate hexahydrate and Cobalt(II) nitrate hexahydrate molar ratio in solution C is 1:2.
6. a kind of preparation method of Cu-Co-S-MOF nanometer sheet according to claim 1, which is characterized in that in step S3, Carbon disulfide and pentamethyl-diethylenetriamine volume ratio are 1:8.3.
7. a kind of preparation method of Cu-Co-S-MOF nanometer sheet according to claim 1, which is characterized in that in step S3, It obtains being immediately placed in reaction kettle after mixed solution D carrying out hydro-thermal reaction, reaction temperature is 150 DEG C, reaction time 8h.
8. a kind of application of the Cu-Co-S-MOF nanometer sheet prepared in claim 1 in electrode material.
CN201910640910.9A 2019-07-16 2019-07-16 A kind of preparation method and applications of Cu-Co-S-MOF nanometer sheet CN110428976A (en)

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