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 PDFInfo
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy 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
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.
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Cited By (5)
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| CN111092222A (en) * | 2019-12-11 | 2020-05-01 | 中南大学 | Cobalt-iron-copper sulfide negative electrode material of sodium ion battery and preparation method thereof |
| CN112103092A (en) * | 2020-07-27 | 2020-12-18 | 浙江工业大学 | Metal cation doped cobalt polysulfide/cobalt hydroxide composite material and preparation method and application thereof |
| CN112885613A (en) * | 2021-01-15 | 2021-06-01 | 上海应用技术大学 | Nano material and preparation method and application thereof |
| CN113363080A (en) * | 2021-05-28 | 2021-09-07 | 上海应用技术大学 | NF @ Co-MOF @ NiMoO4Composite material and preparation method and application thereof |
| CN114524465A (en) * | 2022-01-12 | 2022-05-24 | 河北大学 | Preparation method and application of MOF (Metal organic framework) -derived copper-cobalt bimetallic sulfide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111092222A (en) * | 2019-12-11 | 2020-05-01 | 中南大学 | Cobalt-iron-copper sulfide negative electrode material of sodium ion battery and preparation method thereof |
| CN111092222B (en) * | 2019-12-11 | 2022-01-18 | 中南大学 | Cobalt-iron-copper sulfide negative electrode material of sodium ion battery and preparation method thereof |
| CN112103092A (en) * | 2020-07-27 | 2020-12-18 | 浙江工业大学 | Metal cation doped cobalt polysulfide/cobalt hydroxide composite material and preparation method and application thereof |
| CN112103092B (en) * | 2020-07-27 | 2022-02-11 | 浙江工业大学 | Metal cation doped cobalt polysulfide/cobalt hydroxide composite material and preparation method and application thereof |
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| CN113363080A (en) * | 2021-05-28 | 2021-09-07 | 上海应用技术大学 | NF @ Co-MOF @ NiMoO4Composite material and preparation method and application thereof |
| CN114524465A (en) * | 2022-01-12 | 2022-05-24 | 河北大学 | Preparation method and application of MOF (Metal organic framework) -derived copper-cobalt bimetallic sulfide |
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