CN108281622A - A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube - Google Patents
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube Download PDFInfo
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- CN108281622A CN108281622A CN201711370013.8A CN201711370013A CN108281622A CN 108281622 A CN108281622 A CN 108281622A CN 201711370013 A CN201711370013 A CN 201711370013A CN 108281622 A CN108281622 A CN 108281622A
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- carbon nanotube
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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
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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
- 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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, including the preparation of the functionalization of carbon nanotube, transition metal oxide/carbon nanotube precursor, the preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube.The present invention is compounded to form the hollow ball structure that carbon nanotube embeds transition metal oxide by the carbon nanotube of transition metal oxide and good conductivity, form three-dimensional conductive network, make full use of the height ratio capacity of transition metal oxide and the superior electrical conductivity of carbon nanotube, obtain high magnification, good cycling stability negative material.
Description
Technical field
The invention belongs to technical field of lithium ion battery negative, and in particular to a kind of transition metal oxide/carbon is received
The preparation method of the porous composite negative pole material of mitron.
Background technology
Carbon nanotube（CNTs）It is formed with special hollow reticular structure and with C-C Covalent bonding togethers, and C-C is covalent
Key majority uses sp2 hydridization, has superior mechanical property, while CNTs has that size is small, large specific surface area, good conductivity
Advantage.Also, compared to graphite, lithium ion can be not only embedded in pipe, can also be embedded in ligament, have more embedding lithiums
Position.
The specific capacity of transition metal oxide be far above graphite material, and it is cheap, environmentally safe, have higher
Safety.But there is also very big disadvantages for this material：First, violent volume expansion is generated in charge and discharge process,
Metal oxide dusting, some electrode materials is caused to fall off from collector, battery capacity declines rapidly, the stable circulation of battery
Property is very poor；Secondly, the electron conduction of transition metal oxide is generally very poor, and polarization of electrode is serious in charge and discharge process,
The high rate performance of battery is very poor, the charge/discharge capacity sharp-decay under high current, the two disadvantages significantly limit transition gold
Belong to the commercialization of oxide cathode material.
Invention content
To improve the stable circulation performance and high rate performance of transition metal oxide, the present invention provides a kind of oxo transition metal
The preparation method of the porous composite negative pole material of compound/carbon nanotube is as follows using technical solution：
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, includes the following steps：
（1）The functionalization of carbon nanotube：First, carbon nanotube is disperseed in strong acid；Then, it heats, surfactant is added
Stirring, condensation, reflux, then dilute, it is preserved after then cooling to room temperature centrifuge washing to neutrality；
（2）The preparation of transition metal oxide/carbon nanotube precursor：By transition metal mixtures stirring and dissolving, function is added
Then CNTs after change is added dropwise precipitating reagent reaction in ultrasound in supersonic wave cleaning machine, waits filtration washing after the completion of reacting, then
It is dried to obtain transition metal oxide/carbon nanotube precursor；
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By step（2）In obtain transition gold
Belong to the grinding of oxide/carbon precursor body of Nano tube to be placed in protection gas, transition metal oxide/carbon nanometer is obtained by the reaction in heating
Manage porous composite negative pole material.
Preferably, step（1）The method that middle carbon nanotube is disperseed in strong acid is：Carbon nanotube is dispersed in strong acid,
Disperseed 30 minutes using ultrasonic homogenizer；Step（1）Middle heating is added surfactant stirring, condensation, reflux, then dilutes
Specific method be：Surfactant is added at 20-200 DEG C in scattered material, after being vigorously stirred condensing reflux 1-48h
Stop heating, deionized water dilution is added.
Preferably, the strong acid is any one or more in the concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid.
Preferably, the surfactant is lauryl sodium sulfate, polyethylene glycol, alkyl glycosides, coconut oil diethanol
Any one or more in amide, neopelex.
Preferably, step（1）The method of middle preservation is：CNTs after functionalization is dispersed in by with a certain concentration
It is preserved in ionized water.
Preferably, step（2）In transition metal mixtures be nickel chloride, nickel nitrate, nickel sulfate, cobalt chloride, copper chloride, chlorine
Change any one or more in iron.
Preferably, step（2）In precipitating reagent be ammonium oxalate, sodium carbonate, sodium bicarbonate, one or more of urea.
Preferably, step（2）The weight ratio of middle transition metal mixtures and carbon nanotube is 1:0.01-1:100.
Preferably, step（3）Middle protection gas is one or more of argon gas, nitrogen, air.
Preferably, step（3）The temperature of heating is 200-500 DEG C, heating time 1-6h.
Beneficial effects of the present invention：
（1）Transition metal oxide is compounded to form carbon nanotube by the carbon nanotube with good conductivity and embeds transiting metal oxidation
The hollow ball structure of object forms three-dimensional conductive network, makes full use of the height ratio capacity and carbon nanotube of transition metal oxide
Superior electrical conductivity, obtain high magnification, good cycling stability negative material.
（2）The present invention can effectively improve multiplying power, cycle performance and the stability of transition metal oxide, and can be according to logical
The ratio of control carbon nanotube and transition metal oxide is crossed to adjust the capacity of composite material.
（3）Solvent used in the present invention is water, environmental-friendly and reproducible, of low cost, has preferable scale
Change application potential, industrial prospect is good.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, the present invention is carried out further detailed
Explanation.
Embodiment 1
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, preparation process includes following step
Suddenly：
（1）The functionalization of carbon nanotube：First, by untreated carbon nanotube 200mg dispersion 200ml acid（Concentrated nitric acid and dense
The ratio of hydrochloric acid is 3:1）In, disperseed 30 minutes using ultrasonic homogenizer.Scattered material is added at 80-120 DEG C
20mg surfactants（Surfactant be polyethylene glycol, alkyl glycosides, lauric acid amide of ethanol mixture）, acutely stir
Stop heating after mixing condensing reflux 10-20h, the dilution of 800ml deionized waters is added.Centrifuge washing is then cooled to room temperature to neutrality
Afterwards, finally the CNTs after functionalization is pressed with a certain concentration（10mg/ml）It is evenly dispersed to preserve in deionized water.
（2）The preparation of transition metal oxide/carbon nanotube precursor：By 50mg transition metal mixtures（Nickel nitrate, sulfuric acid
The mixture of nickel, iron chloride, nickel chloride）Stirring and dissolving in deionized water adds the CNTs after functionalization (500ml),
The precipitating reagent of 0.1M is added dropwise in supersonic wave cleaning machine in ultrasound（The mixture of ammonium oxalate, sodium carbonate）150ml reacts 60-
90min, waits filtration washing after the completion of reacting, then in drying box at 20-60 DEG C dry 40-48h obtain transition metal oxide/
Carbon nanotube precursor（Material 1）.
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By the material 1 after drying and grinding
It is placed in tube furnace, in protection gas（Argon gas, nitrogen mixture）Under atmosphere, it is heated to 250-350 DEG C, reacts 3-6h, finally
To the porous composite negative pole material of transition metal oxide/carbon nanotube.
Embodiment 2
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, preparation process includes following step
Suddenly：
（1）The functionalization of carbon nanotube：First, untreated carbon nanotube 300mg is dispersed in 500mL concentrated nitric acids, is made
Disperseed 30 minutes with ultrasonic homogenizer.Lauryl sodium sulfate 40mg is added in scattered material at 20-50 DEG C, acutely
Stop heating after stirring condensing reflux 20-30h, deionized water 1000 ml dilutions are added.Then cool to room temperature centrifuge washing extremely
After neutrality, finally the CNTs after functionalization is pressed with a certain concentration（8mg/ml）It is evenly dispersed to preserve in deionized water.
（2）The preparation of transition metal oxide/carbon nanotube precursor：By nickel chloride, nickel nitrate, nickel sulfate（Nickel chloride,
Nickel nitrate, nickel sulfate weight ratio be 1:2:2）Mixture（1000mg）Stirring and dissolving in deionized water adds function
CNTs (200ml) after change, is added dropwise the sodium bicarbonate of 0.1M in supersonic wave cleaning machine in ultrasound（200ml）, react 100-
120min waits filtration washing after the completion of reacting, then dry 30-35h obtains transiting metal oxidation at 60-80 DEG C in drying box
Object/carbon nanotube precursor（Material 2）.
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By the material 2 after drying and grinding
It is placed in tube furnace, under argon atmosphere, is heated to 200-300 DEG C, reacts 5-6h, finally obtain transition metal oxide/carbon
The porous composite negative pole material of nanotube.
Embodiment 3
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, preparation process includes following step
Suddenly：
（1）The functionalization of carbon nanotube：First, untreated carbon nanotube 100mg is dispersed in the 10mL concentrated sulfuric acids, is used
Ultrasonic homogenizer disperses 30 minutes.Alkyl glycosides, lauric acid amide of ethanol is added in scattered material at 50-80 DEG C
Mixture 5mg, be vigorously stirred after condensing reflux 1-5h and stop heating, deionized water 200 ml dilutions are added.It is subsequently cooled to
After room temperature centrifuge washing to neutrality, finally the CNTs after functionalization is pressed with a certain concentration（1mg/ml）It is dispersed in deionization
It is preserved in water.
（2）The preparation of transition metal oxide/carbon nanotube precursor：By copper chloride, iron chloride（Copper chloride, iron chloride
Weight ratio be 3:1）Mixture（500mg）Stirring and dissolving in deionized water adds the CNTs after functionalization (5ml),
The sodium bicarbonate of 0.1M is added dropwise in ultrasound in supersonic wave cleaning machine（50ml）, 30-60min is reacted, waits mistake after the completion of reacting
Filter washing, then dry 1-10h obtains transition metal oxide/carbon nanotube precursor at 150-200 DEG C in drying box（Material
3）.
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By the material 3 after drying and grinding
It is placed in tube furnace, under nitrogen atmosphere, is heated to 300-350 DEG C, reacts 4-5h, finally obtain transition metal oxide/carbon
The porous composite negative pole material of nanotube.
Embodiment 4
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, preparation process includes following step
Suddenly：
（1）The functionalization of carbon nanotube：First, untreated carbon nanotube 500mg is dispersed in 1000mL concentrated hydrochloric acids, is made
Disperseed 30 minutes with ultrasonic homogenizer.Neopelex, poly- second is added in scattered material at 150-200 DEG C
The mixture 50mg of glycol stops heating after being vigorously stirred condensing reflux 40-48h, and deionized water 2000 ml dilutions are added.So
After postcooling to room temperature centrifuge washing to neutrality, finally the CNTs after functionalization is pressed with a certain concentration（5mg/ml）It is evenly dispersed
It preserves in deionized water.
（2）The preparation of transition metal oxide/carbon nanotube precursor：By cobalt chloride（2000mg）It stirs in deionized water
Dissolving is mixed, the CNTs after functionalization (50ml) is added, the urea of 0.1M is added dropwise in ultrasound in supersonic wave cleaning machine
（500ml）, 120-180min is reacted, waits filtration washing after the completion of reacting, then dry 20-30h at 80-120 DEG C in drying box
Obtain transition metal oxide/carbon nanotube precursor（Material 4）.
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By the material 4 after drying and grinding
It is placed in tube furnace, under nitrogen atmosphere, is heated to 350-450 DEG C, reacts 3-4h, finally obtain transition metal oxide/carbon
The porous composite negative pole material of nanotube.
Embodiment 5
A kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, preparation process includes following step
Suddenly：
（1）The functionalization of carbon nanotube：First, untreated carbon nanotube 350mg is dispersed in 600mL acid（It is the concentrated sulfuric acid, dense
The ratio of hydrochloric acid and concentrated nitric acid is 1:2:3）In, disperseed 30 minutes using ultrasonic homogenizer.By scattered material in 120-
The mixture 30mg of lauryl sodium sulfate and neopelex is added at 150 DEG C, is vigorously stirred condensing reflux 10-
Stop heating after 20h, deionized water 1500 ml dilutions are added.After then cooling to room temperature centrifuge washing to neutrality, finally by work(
CNTs after energyization is pressed with a certain concentration（10mg/ml）It is evenly dispersed to preserve in deionized water.
（2）The preparation of transition metal oxide/carbon nanotube precursor：By cobalt chloride, copper chloride（150mg）In deionization
Stirring and dissolving in water adds the CNTs after functionalization (400ml), is added dropwise 0.1M's in ultrasound in supersonic wave cleaning machine
The mixed liquor of sodium carbonate and sodium bicarbonate（400ml）, 100-120min is reacted, waits filtration washing after the completion of reacting, then in drying
Dry 10-20h obtains transition metal oxide/carbon nanotube precursor at 120-150 DEG C in case（Material 5）.
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By the material 5 after drying and grinding
It is placed in tube furnace, under air atmosphere, is heated to 450-500 DEG C, reacts 1-3h, finally obtain transition metal oxide/carbon
The porous composite negative pole material of nanotube.
The present invention can effectively improve multiplying power, cycle performance and the stability of transition metal oxide, and can be according to passing through
The ratio of carbon nanotube and transition metal oxide is controlled to adjust the capacity of composite material.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
All any modification, equivalent and improvement made by within principle etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the porous composite negative pole material of transition metal oxide/carbon nanotube, which is characterized in that including with
Lower step：
（1）The functionalization of carbon nanotube：First, carbon nanotube is disperseed in strong acid；Then, it heats, surfactant is added
Stirring, condensation, reflux, then dilute, it is preserved after then cooling to room temperature centrifuge washing to neutrality；
（2）The preparation of transition metal oxide/carbon nanotube precursor：By transition metal mixtures stirring and dissolving, function is added
Then CNTs after change is added dropwise precipitating reagent reaction in ultrasound in supersonic wave cleaning machine, waits filtration washing after the completion of reacting, then
It is dried to obtain transition metal oxide/carbon nanotube precursor；
（3）The preparation of the porous composite negative pole material of transition metal oxide/carbon nanotube：By step（2）In obtain transition gold
Belong to the grinding of oxide/carbon precursor body of Nano tube to be placed in protection gas, transition metal oxide/carbon nanometer is obtained by the reaction in heating
Manage porous composite negative pole material.
2. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（1）The method that middle carbon nanotube is disperseed in strong acid is：Carbon nanotube is dispersed in strong acid, is made
Disperseed 30 minutes with ultrasonic homogenizer；Step（1）Surfactant stirring, condensation, reflux is added in middle heating, then diluted
Specific method is：Surfactant is added at 20-200 DEG C in scattered material, is stopped after being vigorously stirred condensing reflux 1-48h
It only heats, deionized water dilution is added.
3. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 2
Method, which is characterized in that the strong acid is any one or more in the concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid.
4. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 2
Method, which is characterized in that the surfactant is lauryl sodium sulfate, polyethylene glycol, alkyl glycosides, coconut oil diethanol acyl
Any one or more in amine, neopelex.
5. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（1）The method of middle preservation is：CNTs after functionalization is dispersed in by with a certain concentration
It is preserved in ionized water.
6. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（2）In transition metal mixtures be nickel chloride, nickel nitrate, nickel sulfate, cobalt chloride, copper chloride, chlorine
Change any one or more in iron.
7. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（2）In precipitating reagent be ammonium oxalate, sodium carbonate, sodium bicarbonate, one or more of urea.
8. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（2）The weight ratio of middle transition metal mixtures and carbon nanotube is 1:0.01-1:100.
9. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（3）Middle protection gas is one or more of argon gas, nitrogen, air.
10. a kind of preparation side of porous composite negative pole material of transition metal oxide/carbon nanotube according to claim 1
Method, which is characterized in that step（3）The temperature of heating is 200-500 DEG C, heating time 1-6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109817939A (en) * | 2019-02-15 | 2019-05-28 | 中科廊坊过程工程研究院 | A kind of cladded type positive electrode, preparation method and application |
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| CN101069928A (en) * | 2007-06-13 | 2007-11-14 | 湖南大学 | Method for preparing copper-base composite particles of internal carbon-inlaid nano pipe |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101069928A (en) * | 2007-06-13 | 2007-11-14 | 湖南大学 | Method for preparing copper-base composite particles of internal carbon-inlaid nano pipe |
Non-Patent Citations (2)
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| AIPING HU等: "Saqima-like Co3O4/CNTs secondary microstructures with ultrahigh initial Coulombic efficiency as an anode for lithium ion batteries", 《J SOLID STATE ELECTROCHEM》 * |
| WEN CAO等: "NiO hollow microspheres interconnected by carbon nanotubes as an anode for lithium ion batteries", 《ELECTROCHIMICA ACTA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109817939A (en) * | 2019-02-15 | 2019-05-28 | 中科廊坊过程工程研究院 | A kind of cladded type positive electrode, preparation method and application |
| CN109817939B (en) * | 2019-02-15 | 2022-05-24 | 廊坊绿色工业技术服务中心 | Coated positive electrode material, and preparation method and application thereof |
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Application publication date: 20180713 |