CN106158423A - A kind of preparation method of carbon nano-fiber composite graphite alkene foam electrode sheet - Google Patents

A kind of preparation method of carbon nano-fiber composite graphite alkene foam electrode sheet Download PDF

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CN106158423A
CN106158423A CN201610674158.6A CN201610674158A CN106158423A CN 106158423 A CN106158423 A CN 106158423A CN 201610674158 A CN201610674158 A CN 201610674158A CN 106158423 A CN106158423 A CN 106158423A
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suspension
carbon nano
described step
reaction
fiber
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肖丽芳
钟玲珑
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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
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • 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
    • H01G11/32—Carbon-based
    • 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
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • 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 provides the preparation method of a kind of carbon nano-fiber composite graphite alkene foam electrode sheet, including following step: step (1) joins ball milling in ball mill by fine to graphite oxide and polypropylene, then the mixture after ball milling is joined ethanol and ultrasonic disperse in the mixed solution of water, forms suspension；Nickel foam is soaked in above-mentioned suspension by step (2), solvent evaporated, places into the Muffle reaction in furnace of hydrogen nitrogen mixed gas protection, natural cooling after reaction completely；Above-mentioned product be impregnated in hydrochloric acid by step (3), reaction, obtains foamy graphite alkene after reaction completely；Carbon nano-fiber is joined in dehydrated alcohol by step (4), is ultrasonically formed suspension, then the alcohol suspension titration containing carbon nano-fiber is applied on foamy graphite alkene, is dried, and after cooling, Kun pressure obtains electrode slice.Electrode slice prepared by the method need not, as adding binding agent and conductive agent in conventional electrodes sheet, reduce the cost of material.

Description

A kind of preparation method of carbon nano-fiber composite graphite alkene foam electrode sheet
Technical field
The invention belongs to supercapacitor technologies field, particularly relate to a kind of carbon nano-fiber composite graphite alkene foam electricity The preparation method of pole piece.
Background technology
Graphene is a kind of Novel Carbon Nanomaterials, by monolayer sp2 carbon atom tightly packed one-tenth bi-dimensional cellular shape structure. Graphene has electricity, calorifics, optics and the mechanical property of excellence.The theoretical specific surface area that Graphene is high simultaneously and excellent electricity Conductance determines it as electrode material in the great potential of electrochemical energy storing device.
The two-dimensional structure of Graphene uniqueness and outstanding physical characteristic so that it is the application in ultracapacitor has greatly Ground potentiality.Compared with tradition Dare porous carbon materials, Graphene has the highest electric conductivity, big specific surface area and substantial amounts of Interlayer constructs, thus becomes the selection of the more promising electrode material of double layer capacitor.But Graphene is in preparation process It is susceptible to stacking, affects grapheme material dispersibility in the electrolyte and surface wettability, reduce grapheme material Effective ratio area and electrical conductivity.Therefore, it is to avoid Graphene stacking is to prepare high-energy-density and high power density Graphene The technical barrier of ultracapacitor.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation of a kind of carbon nano-fiber composite graphite alkene foam electrode sheet Method, high-specific surface area, high connductivity grapheme foam compound electric pole piece prepared by the method both can serve as collector, the most permissible Serve as active material, the capacity of electrode can be increased again after load carbon nano-fiber, ultracapacitor can also be simplified simultaneously The technical process of preparation, reduces its process costs.
The present invention provides the preparation method of a kind of carbon nano-fiber composite graphite alkene foam electrode sheet to be:
Step (1) joins ball milling 30-60min in ball mill, then by the mixing after ball milling by fine to graphite oxide and polypropylene Thing joins ethanol and ultrasonic disperse in the mixed solution of water, forms the suspension of concentration 1-20g/L.
Nickel foam is soaked 10-60min, solvent evaporated in above-mentioned suspension by step (2), places into hydrogen nitrogen mixed gas and protects 800-1100 DEG C of reaction 1-10h, natural cooling after reaction completely in the Muffle furnace protected.
Above-mentioned product be impregnated in the hydrochloric acid of 1-3mol/L by step (3), and 60-80 DEG C of reaction 5-10h, after reaction completely Obtain foamy graphite alkene.
Carbon nano-fiber is joined in dehydrated alcohol by step (4), and ultrasonic 10-30min forms suspension, then will be containing receiving The alcohol suspension titration of rice carbon fiber is applied on foamy graphite alkene, is dried, and after cooling, Kun pressure obtains electrode slice.
Further, in described step (1), Ball-milling Time is 30-60min；
Further, the 0.01-5% that quality is graphite oxide quality that in described step (1), polypropylene is fine；
Further, in described step (1), in the mixed solution of ethanol and water, the volume ratio of ethanol and water is 0.25-4；
Further, described step (1) is at the suspension that concentration is 1-20g/L of graphite oxide suspension；
Further, in described step (2), nickel foam is immersed in the time in graphite oxide suspension is 10-60min；
Further, in described step (2), the atmosphere in Muffle furnace is the hydrogen nitrogen mixed gas containing 5% hydrogen；
Further, the described step (2) reaction temperature in Muffle furnace is 800-1100 DEG C, and the response time is 1-10h；
Further, in described step (3), concentration of hydrochloric acid is 1-3mol/L；
Further, the described step (3) reaction temperature in hydrochloric acid is 60-80 DEG C, and the response time is 5-10h；
Further, in described step (4), the mass concentration of carbon nano-fiber alcohol suspension is 30-70%；
Further, in described step (4), ultrasonic time is 10-30min；
Further, the thickness of the electrode slice obtained in described step (4) is 100-500um.
There is advantages that (1) high-specific surface area, high conductivity grapheme foam both as collector Again as active material, simplify preparation technology, reduce cost；(2) Graphene and Nano carbon fibers after carbon nano-fiber load Dimension can play capacity, can be effectively increased the capacity of electrode；(3) loose structure of grapheme foam can provide effective Electronics and ion conduction channel, it is achieved high-energy-density and high power density；(4) electrode slice prepared by the method need not as often Rule electrode slice adds binding agent and conductive agent, reduces the cost of material.
Accompanying drawing explanation
Fig. 1 is preparation technology flow chart of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the preferably embodiment of the present invention is described in further detail:
Embodiment 1
(1) ball milling 30min in ball mill is joined, then by mixing after ball milling by fine to 10g graphite oxide and 0.001g polypropylene Compound joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 0.25, forms the suspension of concentration 1g/L.
(2) nickel foam is soaked in above-mentioned suspension 10min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen 800 DEG C of reaction 10h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 1mol/L, 60 DEG C of reaction 10h, obtain foam stone after reaction completely Ink alkene.
(4) joining in dehydrated alcohol by carbon nano-fiber, it is 30% suspension that ultrasonic 10min forms mass concentration, then will Alcohol suspension titration containing carbon nano-fiber is applied on foamy graphite alkene, is dried, and is then placed in Muffle furnace 200 DEG C and moves back Fire 60min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor Device.
Embodiment 2
(1) ball milling 60min in ball mill is joined, then by the mixing after ball milling by fine to 10g graphite oxide and 0.5g polypropylene Thing joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 4, forms the suspension of concentration 20g/L.
(2) nickel foam is soaked in above-mentioned suspension 60min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen 1100 DEG C of reaction 1h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 3mol/L, 80 DEG C of reaction 5h, obtain foam stone after reaction completely Ink alkene.
(4) joining in dehydrated alcohol by carbon nano-fiber, it is 70% suspension that ultrasonic 10-30min forms mass concentration, Again the alcohol suspension containing carbon nano-fiber is titrated and be applied on foamy graphite alkene, be dried, be then placed in Muffle furnace 300 DEG C annealing 30min, after cooling Kun pressure obtain electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor Device.
Embodiment 3
(1) ball milling 45min in ball mill is joined, then by the mixing after ball milling by fine to 10g graphite oxide and 0.1g polypropylene Thing joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 0.5, forms the suspension of concentration 3g/L.
(2) nickel foam is soaked in above-mentioned suspension 30min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen 900 DEG C of reaction 5h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 2mol/L, 75 DEG C of reaction 7h, obtain foamy graphite after reaction completely Alkene.
(4) joining in dehydrated alcohol by carbon nano-fiber, it is 50% suspension that ultrasonic 20min forms mass concentration, then will Alcohol suspension titration containing carbon nano-fiber is applied on foamy graphite alkene, is dried, and is then placed in Muffle furnace 250 DEG C and moves back Fire 450min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor Device.
Embodiment 4
(1) ball milling 40min in ball mill is joined, then by the mixture after ball milling by fine to 10g graphite oxide and 3g polypropylene Join ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 2, form the suspension of concentration 10g/L.
(2) nickel foam is soaked in above-mentioned suspension 50min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen 1000 DEG C of reaction 3h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 1.5mol/L, 65 DEG C of reaction 9h, obtain foam stone after reaction completely Ink alkene.
(4) joining in dehydrated alcohol by carbon nano-fiber, it is 50% suspension that ultrasonic 15min forms mass concentration, then will Alcohol suspension titration containing carbon nano-fiber is applied on foamy graphite alkene, is dried, and is then placed in Muffle furnace 220 DEG C and moves back Fire 40min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor Device.
Embodiment 5
(1) ball milling 40min in ball mill is joined, then by the mixture after ball milling by fine to 10g graphite oxide and 1g polypropylene Join ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 1, form the suspension of concentration 5g/L.
(2) nickel foam is soaked in above-mentioned suspension 20min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen 950 DEG C of reaction 80h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 2.5mol/L, 75 DEG C of reaction 4h, obtain foam stone after reaction completely Ink alkene.
(4) joining in dehydrated alcohol by carbon nano-fiber, it is 60% suspension that ultrasonic 25min forms mass concentration, then will Alcohol suspension titration containing carbon nano-fiber is applied on foamy graphite alkene, is dried, and is then placed in Muffle furnace 280 DEG C and moves back Fire 35min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor Device.
Preparation method is as it is shown in figure 1, its effect is as shown in table 1, as shown in Table 1: patent system of the present invention is for electrode slice quality Specific capacity has reached 290.2-299.7 F/g.
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Specific discharge capacity (F/g) 290.2 299.7 292.1 293.6 294.5
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert this Bright being embodied as is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the protection of the present invention Scope.

Claims (10)

1. the preparation method of a carbon nano-fiber composite graphite alkene foam electrode sheet, it is characterised in that include following step Rapid:
Step (1) joins ball milling in ball mill by fine to graphite oxide and polypropylene, is then joined by the mixture after ball milling Ethanol and ultrasonic disperse in the mixed solution of water, form suspension；
Nickel foam is soaked in above-mentioned suspension by step (2), solvent evaporated, places in the Muffle furnace of hydrogen nitrogen mixed gas protection Reaction, natural cooling after reaction completely；
Above-mentioned product be impregnated in hydrochloric acid by step (3), reaction, obtains foamy graphite alkene after reaction completely；
Carbon nano-fiber is joined in dehydrated alcohol by step (4), is ultrasonically formed suspension, then by the second containing carbon nano-fiber The titration of alcohol suspension is applied on foamy graphite alkene, is dried, and after cooling, Kun pressure obtains electrode slice.
2. the method for claim 1, it is characterised in that in described step (1), Ball-milling Time is 30-60min.
3. the method for claim 1, it is characterised in that the quality that in described step (1), polypropylene is fine is graphite oxide The 0.01-5% of quality.
4. the method for claim 1, it is characterised in that ethanol and ethanol in the mixed solution of water in described step (1) It is 0.25-4 with the volume ratio of water.
5. the method for claim 1, it is characterised in that described step (1) is 1-in the concentration of graphite oxide suspension The suspension of 20g/L.
6. the method for claim 1, it is characterised in that in described step (2), nickel foam is immersed in graphite oxide suspension Time in liquid is 10-60min.
7. the method for claim 1, it is characterised in that in described step (2), the atmosphere in Muffle furnace is dense containing volume Spend the hydrogen nitrogen mixed gas of 5% hydrogen；Reaction temperature in Muffle furnace is 800-1100 DEG C, and the response time is 1-10h.
8. the method for claim 1, it is characterised in that in described step (3), concentration of hydrochloric acid is 1-3mol/L；At hydrochloric acid In reaction temperature be 60-80 DEG C, the response time is 5-10h.
9. the method for claim 1, it is characterised in that the matter of carbon nano-fiber alcohol suspension in described step (4) Amount concentration is 30-70%；Ultrasonic time is 10-30min.
10. the method for claim 1, it is characterised in that the thickness of the electrode slice obtained in described step (4) is 100- 500um。
CN201610674158.6A 2016-08-16 2016-08-16 A kind of preparation method of carbon nano-fiber composite graphite alkene foam electrode sheet Pending CN106158423A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108054028A (en) * 2017-11-03 2018-05-18 佛山科学技术学院 A kind of preparation method of foam electrode piece

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103545121A (en) * 2013-10-23 2014-01-29 南京大学 Supercapacitor electrode material preparation method based on three-dimensional graphene
CN104008888A (en) * 2014-06-13 2014-08-27 上海利物盛企业集团有限公司 Preparation method of composite material and electrode slice for super capacitor
CN104495811A (en) * 2014-12-12 2015-04-08 盐城市新能源化学储能与动力电源研究中心 Graphene composite material and preparation method thereof
US20160086740A1 (en) * 2014-09-24 2016-03-24 Southwest University Multi-layer based new conceptual battery type supercapacitor with high power density and high energy density and method for preparing the same
CN105609736A (en) * 2016-02-21 2016-05-25 钟玲珑 Preparation method for three-dimensional carbon nanotube/nitrogen-doped graphene/sulfur electrode slice

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103545121A (en) * 2013-10-23 2014-01-29 南京大学 Supercapacitor electrode material preparation method based on three-dimensional graphene
CN104008888A (en) * 2014-06-13 2014-08-27 上海利物盛企业集团有限公司 Preparation method of composite material and electrode slice for super capacitor
US20160086740A1 (en) * 2014-09-24 2016-03-24 Southwest University Multi-layer based new conceptual battery type supercapacitor with high power density and high energy density and method for preparing the same
CN104495811A (en) * 2014-12-12 2015-04-08 盐城市新能源化学储能与动力电源研究中心 Graphene composite material and preparation method thereof
CN105609736A (en) * 2016-02-21 2016-05-25 钟玲珑 Preparation method for three-dimensional carbon nanotube/nitrogen-doped graphene/sulfur electrode slice

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108054028A (en) * 2017-11-03 2018-05-18 佛山科学技术学院 A kind of preparation method of foam electrode piece

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Application publication date: 20161123