CN103762366A - Preparation method of carbon nanotube composite electrode - Google Patents

Preparation method of carbon nanotube composite electrode Download PDF

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Publication number
CN103762366A
CN103762366A CN201310604266.2A CN201310604266A CN103762366A CN 103762366 A CN103762366 A CN 103762366A CN 201310604266 A CN201310604266 A CN 201310604266A CN 103762366 A CN103762366 A CN 103762366A
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carbon nano
electrode
preparation
tubes
manganese acetate
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CN201310604266.2A
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CN103762366B (en
Inventor
范茂松
金翼
官亦标
马小航
丁楚雄
陈春华
来小康
郭剑波
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University of Science and Technology of China USTC
State Grid Corp of China SGCC
China Electric Power Research Institute Co Ltd CEPRI
State Grid Anhui Electric Power Co Ltd
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University of Science and Technology of China USTC
State Grid Corp of China SGCC
China Electric Power Research Institute Co Ltd CEPRI
State Grid Anhui Electric Power Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a preparation method of a carbon nanotube composite electrode, wherein the method comprises the following steps: (1) preparing a manganese acetate solution; (2) performing pretreatment of multi-wall carbon nanotubes; (3) preparing a precursor solution by pouring the manganese acetate solution into the multi wall carbon nanotubes; (4) regulating DC voltage and the substrate temperature for depositing on a substrate, before the deposition, introducing nitrogen in advance, after a film is prepared, sintering in nitrogen atmosphere to prepare the manganese oxide / multi-wall carbon nanotube composite film electrode. The preparation method realizes preparation of the manganese oxide / multi-wall carbon nanotube composite electrode, and can prepare electrodes with different carbon nanotube addition proportion; by the electrode prepared by the preparation method, the use of other conductive carbon materials and current collectors in batteries can be reduced, the use cost of the carbon nanotubes in the batteries can be reduced, the electrode prepared by the preparation method is lighter in mass, the electrode energy density can be enhanced, the electrode prepared by the preparation method is better in electrode conductivity, and the application field of the electrode is broadened.

Description

A kind of carbon nano-tube combination electrode preparation method
Technical field
The invention belongs to battery energy storage technology, specifically relate to a kind of carbon nano-tube combination electrode preparation method.
Background technology
Within 1997, there is short commentary article to point out that carbon nano-tube can apply in lithium ion battery electrode material, and just having occurred for 1999 after 2 years really using carbon nano-tube as lithium ion battery negative material, replace the research of conventional material with carbon element, so far after, the application of carbon nano-tube in lithium-ion battery system entered the fast-developing stage, from the early stage negative material that directly does, use, arrive as positive electrode and cathode material conductive agent or conductive additive use, or as using without collector electrode substrate, research is up to date found by carbon nano-tube being carried out to the modification of specific functional groups, carbon nano-tube can be used as equally a kind of special positive electrode and uses.
The not same-action that carbon nano-tube is brought into play in lithium-ion battery system, first be as conductive agent or conductive agent additive, why carbon nano-tube can be applied as conductive component, mainly by its peculiar physical property, determined, carbon nano-tube is with respect to other conductive carbon materials, have higher conductance, indoor temperature measurement can reach 5 × 105 s/ m, simultaneously as a kind of special monodimension nanometer material, it has very high draw ratio (>10000), mean under less mixed ratio, can be just that electrode material obtains good conductive effect, for other conductive carbon materials, can effectively reduce conductive agent consumption, thereby indirectly improve the load capacity of active material in unit volume, and then improve the energy of monomer lithium ion battery.And carbon nano-tube has the characteristic of chirality π Orbital Overlap, when transmitting therein, can radially with micron-sized mean free path, transmit along it electronics, this characteristic can active electrode material high rate performance, for practical application tool, have very important significance.In conductive agent application aspect, carbon nano-tube can apply to different electrode materials, as LiCoO in positive electrode 2, LiMn 2o 4, LiNi 0.8co 0.2o 2, LiFePO 4, Li 3v 2(PO 4) 3, LiNi 0.45al 0.05mn 1.5o 4, LiCo 0.5mn 0.5pO 4deng, as Co in negative material 3o 4, CoO, Li 4ti 5o 12, SnO 2, CoFe 2o 4deng, no matter, for positive electrode or negative material, carbon nano-tube is introduced and wherein can be formed good conductive network as conductive agent, is conducive to the transmission of electronics, therefore the electrode material of preparation often has excellent large high rate performance, and long cyclical stability is also improved.
The another kind of form that carbon nano-tube is used as conductive agent is done exactly without collector combination electrode, without collector electrode, be not there is no collector, but utilize film prepared by carbon nano-tube to replace conventional collector (Copper Foil or aluminium foil), the main implementation of this form is compounded in electrode material among carbon nano-tube film exactly, carbon nano-tube film also can be used as collector when serving as conductive agent like this, therefore can reduce the use of other conductive carbon materials and conventional collector, and it is better that Film laminated electrode has conductivity with respect to conventional collector electrode, quality is lighter, the better feature of pliability, application that can open lithium ion battery, the more important thing is with respect to conventional lithium ion battery, in the battery unit volume of Film laminated, contained active material quality improves, cell integrated energy density also obviously improves.
Except utilizing its conduction property, appearing at the earliest in lithium ion battery of carbon nano-tube used directly to replace conventional material with carbon element as negative material, with respect to conventional graphite cathode, its theoretical specific capacity of carbon nanometer tube negative pole material exceedes 1116mAh/g, much larger than the 372mAh/g of graphite cathode, so high capacity is mainly because except the carbocyclic ring storage of carbon nano-tube lithium own, there are a large amount of defects in its tubular structure, the position of removal lithium embedded can be provided, and also can store up lithium between carbon nano-tube carbon-coating.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of carbon nano-tube combination electrode preparation method, the method is take manganese acetate and multi-walled carbon nano-tubes as raw material, by electrostatic spray precipitation equipment, grope the parameter control in preparation process, successfully prepared manganese acetate/multi-walled carbon nano-tubes combination electrode.It is better that this Film laminated electrode has conductivity with respect to conventional collector electrode, quality is lighter, the better feature of pliability, application that can open lithium ion battery, simultaneously, with respect to conventional lithium ion battery, in the battery unit volume of Film laminated, contained active material quality improves, and cell integrated energy density also obviously improves.
The object of the invention is to adopt following technical proposals to realize:
A kind of carbon nano-tube combination electrode preparation method, its improvements are, described method comprises:
(1) preparation manganese acetate solution;
(2) multi-walled carbon nano-tubes is carried out to preliminary treatment;
(3) pour described manganese acetate solution into multi-walled carbon nano-tubes and make precursor liquid;
(4) regulate direct voltage and underlayer temperature, on substrate, deposit, deposition starts front pre-logical nitrogen, carries out sintering after preparing film under nitrogen atmosphere, makes manganese oxide/multi-walled carbon nano-tubes composite film electrode.
Preferably, described step (1) comprises take 1.2-propylene glycol as solvent, manganese acetate is dissolved in 1.2-propylene glycol solvent and adds thermal agitation at 65 ℃.
Preferably, described step (2) comprises take the concentrated sulfuric acid and red fuming nitric acid (RFNA) mixed solution as cleaning fluid, at 65 ℃, stirs back and heats up in a steamer, standby after eccentric cleaning, for improving the dispersiveness of multi-walled carbon nano-tubes at water.
Further, in the described concentrated sulfuric acid and red fuming nitric acid (RFNA) mixed solution, be chosen as the concentrated sulfuric acid and red fuming nitric acid (RFNA) volume ratio 1:1.
Preferably, described step (3) comprises the multi-walled carbon nano-tubes after cleaning is dispersed in deionized water, carries out ultrasonic dispersion, is poured in described manganese acetate solution, stirs after ultrasonic and makes precursor liquid.
Further, in described precursor liquid, the concentration of manganese acetate is 5-15mM, and the additional proportion of multi-walled carbon nano-tubes is to take with the percentage of manganese acetate quality used, and the adding proportion of selecting is being respectively between 0wt%～20wt%.
Preferably, described step (4) comprises that adopting nickel foam is substrate, regulate direct voltage and underlayer temperature, after voltage and temperature reach, described precursor liquid deposits on substrate, and deposition starts front pre-logical nitrogen, in whole process, keeps nitrogen atmosphere, after preparing film, under nitrogen atmosphere, carry out sintering, make manganese oxide/multi-walled carbon nano-tubes composite film electrode.
Compared with the prior art, beneficial effect of the present invention is:
1, the present invention has realized the preparation of manganese oxide/multi-walled carbon nano-tubes combination electrode, can prepare the electrode of different carbon nano-tube adding proportions.
2, the electrode that prepared by the present invention has reduced the use of other conductive carbon material and collector in battery, can lower the use cost of carbon nano-tube in battery.
3, the electrode quality that prepared by the present invention is lighter, has improved the energy density of electrode.
4, the electrode conductivuty that prepared by the present invention is better, has widened the application of electrode.
Accompanying drawing explanation
Fig. 1 is a kind of carbon nano-tube combination electrode preparation method schematic diagram provided by the invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
The manganese source that preparation process is used is manganese acetate Mn (Ac) 2.4H 2o, take multi-walled carbon nano-tubes as carbon source, electrostatic spray depositing device used be the exploitation of laboratory designed, designed can the lower work of nitrogen atmosphere protection sprayer unit, device is as shown in Figure 1.
Specific experiment flow process is as follows:
(1) take 1.2-propylene glycol as solvent, first manganese acetate is dissolved in 1.2-propylene glycol solvent at 65 ℃, then add thermal agitation.
(2) multi-walled carbon nano-tubes is first carried out to preliminary treatment, take the concentrated sulfuric acid and red fuming nitric acid (RFNA) mixed solution as cleaning fluid, at 65 ℃, stir back and heat up in a steamer, standby after eccentric cleaning, to improve the dispersiveness of multi-walled carbon nano-tubes in water.
(3) multi-walled carbon nano-tubes after cleaning is dispersed in deionized water, carry out ultrasonic dispersion, be poured into again the above-mentioned manganese acetate solution preparing, stir ultrasonic, make precursor liquid, in final precursor liquid, the concentration of manganese acetate is 5-15mM, and the additional proportion of multi-walled carbon nano-tubes is to take with the percentage of manganese acetate quality used, and the adding proportion of selecting is being respectively between 0wt%～20wt%.
(4) take nickel foam as substrate, regulate direct voltage and underlayer temperature, after voltage and temperature reach, precursor liquid deposits on substrate, deposition starts front pre-logical nitrogen, in whole process, keep nitrogen atmosphere, under nitrogen atmosphere, carry out sintering after preparing film, make manganese oxide/multi-walled carbon nano-tubes composite film electrode.
Embodiment
(1) take 1.2-propylene glycol as solvent, first manganese acetate is dissolved at 65 ℃ to (50ml) in 1.2-propylene glycol solvent, add thermal agitation 2 hours.
(2) multi-walled carbon nano-tubes is first carried out to preliminary treatment, take the concentrated sulfuric acid and red fuming nitric acid (RFNA) (volume ratio 1:1) mixed solution as cleaning fluid, stir back at 65 ℃ and heat up in a steamer 10 hours, standby after eccentric cleaning, to improve the dispersiveness of multi-walled carbon nano-tubes in water.
(3) multi-walled carbon nano-tubes after cleaning is dispersed in to (10ml) in deionized water, ultrasonic dispersion 0.5 hour, be poured into again the above-mentioned manganese acetate solution preparing, stir ultrasonic each 0.5 hour, make precursor liquid, in final precursor liquid, the concentration of manganese acetate is 10mM, and the additional proportion of multi-walled carbon nano-tubes is to take with the percentage of manganese acetate quality used, and the adding proportion of selecting is 5wt%.
(4) take nickel foam as substrate, direct voltage～8.5KV, underlayer temperature is 250 ℃, sedimentation time is 2.5 hours, deposition starts front pre-logical nitrogen 30 minutes, keeps nitrogen atmosphere in experimentation, prepares after film at 500 ℃, sintering 5 hours under nitrogen atmosphere, makes manganese oxide/multi-walled carbon nano-tubes composite film electrode.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit, although the present invention is had been described in detail with reference to above-described embodiment, those of ordinary skill in the field are to be understood that: still can modify or be equal to replacement the specific embodiment of the present invention, and do not depart from any modification of spirit and scope of the invention or be equal to replacement, it all should be encompassed in the middle of claim scope of the present invention.

Claims (7)

1. a carbon nano-tube combination electrode preparation method, is characterized in that, described method comprises:
(1) preparation manganese acetate solution;
(2) multi-walled carbon nano-tubes is carried out to preliminary treatment;
(3) pour described manganese acetate solution into multi-walled carbon nano-tubes and make precursor liquid;
(4) regulate direct voltage and underlayer temperature, on substrate, deposit, deposition starts front pre-logical nitrogen, carries out sintering after preparing film under nitrogen atmosphere, makes manganese oxide/multi-walled carbon nano-tubes composite film electrode.
2. a kind of carbon nano-tube combination electrode preparation method as claimed in claim 1, is characterized in that, described step (1) comprises take 1.2-propylene glycol as solvent, manganese acetate is dissolved in 1.2-propylene glycol solvent and adds thermal agitation at 65 ℃.
3. a kind of carbon nano-tube combination electrode preparation method as claimed in claim 1, it is characterized in that, described step (2) comprises take the concentrated sulfuric acid and red fuming nitric acid (RFNA) mixed solution as cleaning fluid, at 65 ℃, stirs back and heat up in a steamer, standby after eccentric cleaning, for improving the dispersiveness of multi-walled carbon nano-tubes at water.
4. a kind of carbon nano-tube combination electrode preparation method as claimed in claim 3, is characterized in that, is chosen as the concentrated sulfuric acid and red fuming nitric acid (RFNA) volume ratio 1:1 in the described concentrated sulfuric acid and red fuming nitric acid (RFNA) mixed solution.
5. a kind of carbon nano-tube combination electrode preparation method as claimed in claim 1, it is characterized in that, described step (3) comprise by clean after multi-walled carbon nano-tubes be dispersed in deionized water, carry out ultrasonic dispersion, be poured in described manganese acetate solution, stir after ultrasonic and make precursor liquid.
6. a kind of carbon nano-tube combination electrode preparation method as claimed in claim 5, it is characterized in that, in described precursor liquid, the concentration of manganese acetate is 5-15mM, the additional proportion of multi-walled carbon nano-tubes is to take with the percentage of manganese acetate quality used, and the adding proportion of selecting is being respectively between 0wt%～20wt%.
7. a kind of carbon nano-tube combination electrode preparation method as claimed in claim 1, it is characterized in that, described step (4) comprises that adopting nickel foam is substrate, regulate direct voltage and underlayer temperature, after voltage and temperature reach, described precursor liquid deposits on substrate, deposition starts front pre-logical nitrogen, in whole process, keep nitrogen atmosphere, under nitrogen atmosphere, carry out sintering after preparing film, make manganese oxide/multi-walled carbon nano-tubes composite film electrode.
CN201310604266.2A 2013-11-25 2013-11-25 A kind of carbon nano-tube combination electrode preparation method Active CN103762366B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109830649A (en) * 2019-01-14 2019-05-31 湘潭大学 A kind of preparation process of long circulation life, height ratio capacity flexible electrode

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060061412A (en) * 2004-12-02 2006-06-08 현대자동차주식회사 Method for manufacturing manganese oxide/carbon nanotube composite electrode for super capacitor using electrostatic spary deposition
CN1790783A (en) * 2004-11-26 2006-06-21 三星Sdi株式会社 Electrode for fuel cell, fuel cell comprising the same, and method for preparing the same
US7986509B2 (en) * 2008-01-17 2011-07-26 Fraser Wade Seymour Composite electrode comprising a carbon structure coated with a thin film of mixed metal oxides for electrochemical energy storage
US8493711B2 (en) * 2008-01-17 2013-07-23 Fraser W. SEYMOUR Monolithic electrode, related material, process for production, and use thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1790783A (en) * 2004-11-26 2006-06-21 三星Sdi株式会社 Electrode for fuel cell, fuel cell comprising the same, and method for preparing the same
KR20060061412A (en) * 2004-12-02 2006-06-08 현대자동차주식회사 Method for manufacturing manganese oxide/carbon nanotube composite electrode for super capacitor using electrostatic spary deposition
US7986509B2 (en) * 2008-01-17 2011-07-26 Fraser Wade Seymour Composite electrode comprising a carbon structure coated with a thin film of mixed metal oxides for electrochemical energy storage
US8493711B2 (en) * 2008-01-17 2013-07-23 Fraser W. SEYMOUR Monolithic electrode, related material, process for production, and use thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109830649A (en) * 2019-01-14 2019-05-31 湘潭大学 A kind of preparation process of long circulation life, height ratio capacity flexible electrode
CN109830649B (en) * 2019-01-14 2021-10-26 湘潭大学 Preparation process of flexible electrode with long cycle life and high specific capacity

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