CN110416509A - A kind of lithium ion battery negative material of height ratio capacity and preparation method thereof - Google Patents
A kind of lithium ion battery negative material of height ratio capacity and preparation method thereof Download PDFInfo
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- CN110416509A CN110416509A CN201910646766.XA CN201910646766A CN110416509A CN 110416509 A CN110416509 A CN 110416509A CN 201910646766 A CN201910646766 A CN 201910646766A CN 110416509 A CN110416509 A CN 110416509A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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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 present invention relates to lithium ion battery negative materials of a kind of height ratio capacity and preparation method thereof.The lithium ion battery negative material is that echinus-like carbon coats cobalt/cobalt oxide, using chlorination cobalt precursor, sea urchin shape cobaltosic oxide is prepared by hydrothermal synthesis, then Carbon deposition is carried out by vapour deposition process, echinus-like carbon cladding cobalt/cobalt oxide composite lithium ion battery cathode material is prepared.It is overall electrode material with electric by carbon coating, and improve structural stability of the sea urchin shape cobaltosic oxide in charge and discharge process using cobaltosic oxide as active material.Also, in vapor deposition processes under the action of hydrogen, the cobalt valence state of sea urchin shape cobaltosic oxide can change, and the cobalt of mixed valence can provide additional electric conductivity for electrode material.
Description
Technical field
The present invention relates to lithium ion battery negative materials of a kind of height ratio capacity and preparation method thereof, belong to materials chemistry neck
Domain.
Background technique
21 century economy and science and technology are fast-developing, but limited petroleum, coal on the main source or the earth of the energy
With the fossil fuels such as natural gas.It is well known that being brought tight derived from the gaseous contamination atmosphere that fossil fuel and biomass fuel discharge
The global problems of weight.In face of increasingly serious energy and environmental problem, developing reproducible clean energy resource, oneself compels to be essential through becoming
It solves the problems, such as.New energy refers to the unconventional energy resource developed and used on the basis of new technology, including wind energy, solar radiation
Energy, ocean energy, geothermal energy, biomass energy, ammonia energy and nuclear energy etc..New forms of energy resource potentiality are big, can continuous utilization, meeting the energy
Demand improves that energy resource structure, reducing environmental pollution, promote economic development etc. has played important function.However, wind energy,
The electric power that the new energies such as solar energy issue has unstability and discontinuity, it is difficult to directly apply to production and living.Therefore,
Efficient energy storage and energy conversion device are established, to unstable power collection be got up and can be in due course by it
Steady release, has great importance for the development and utilization of new energy.
Compared with other rechargeable batteries (such as lead-acid battery, nickel-metal hydride battery), lithium ion battery has specific capacity height, circulation
Service life length, voltage platform height, memory-less effect, fast charging and discharging, security performance are high, self-discharge rate is low, environmental pollution is small, body
The apparent advantages such as long-pending small and light weight.Currently, lithium ion battery has been widely used for mobile phone, camera, laptop
Equal small size digitals equipment, and just sent out towards the energy-storage battery direction of the electric vehicle battery and wind energy of enlargement and solar energy
Exhibition.More stringent requirements are proposed for performance of the demand to lithium ion battery as energy-storage battery, and the weight as lithium ion battery
Component part is wanted, positive and negative pole material is the key factor for determining its performance.Therefore, the lithium of high-performance, low cost is researched and developed
Ion battery electrode materials, which seem, to become more and more important.
Summary of the invention
Reversible capacity is smaller, cycle performance is poor present in negative electrode material of the present invention for current lithium ion battery etc.
Problem provides a kind of lithium ion battery negative material and preparation method thereof of height ratio capacity.The lithium-ion electric of the height ratio capacity
Pond negative electrode material is a kind of echinus-like carbon cladding cobalt/cobalt oxide, is then to pass through gas phase by first preparing sea urchin shape cobaltosic oxide
Sedimentation carries out Carbon deposition, and echinus-like carbon cladding cobalt/cobalt oxide composite lithium ion battery cathode material is prepared.
The present invention solves technical solution used by the technical problem:
A kind of preparation method of height ratio capacity lithium ion battery negative material, the lithium ion battery negative material are sea urchin
Shape carbon coating cobalt oxide, preparation process the following steps are included:
(1) sea urchin shape cobaltosic oxide is prepared:
Cobalt chloride, urea are dissolved in deionized water, mixed liquor is placed in reaction kettle after magnetic agitation is uniform and carries out water
Thermal response, natural cooling after hydro-thermal reaction, respectively washs three times product using deionized water and ethyl alcohol, product is placed in baking oven
In 60 DEG C of dryings, desciccate is placed in Muffle furnace calcining and obtains sea urchin shape cobaltosic oxide.
(2) echinus-like carbon cladding cobalt/cobalt oxide is prepared:
The sea urchin shape cobaltosic oxide powder being prepared in step (1) is placed in tube furnace, is risen under an argon atmosphere
Temperature is passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant to 500~700 DEG C, after being continually fed into 1~3min, closes
Hydrogen and acetylene, natural cooling, obtains echinus-like carbon cladding cobalt/cobalt oxide composite material under an argon atmosphere.
Preferably, in step (1), the usage ratio of cobalt chloride, urea and deionized water are as follows: (0.1~0.5) g:(1~5)
G:(10~100) mL.
Preferably, in step (1), the magnetic agitation time is 1~3h.
Preferably, in step (1), the temperature of the hydro-thermal reaction is 100~150 DEG C, the hydro-thermal reaction time is 12~
24h。
Preferably, in step (1), the temperature of the calcining is 200~400 DEG C, calcination time 6-12h
Preferably, in step (2), the quality of sea urchin shape cobaltosic oxide powder is 0.1~0.5g, hydrogen flow rate 100
~300mL/min, acetylene flow velocity are 10~50mL/min.
Preferably, after acetylene and hydrogen gas mixture are continually fed into 1~3min in step (2), stopping acetylene first is passed through,
Acetylene stopping is passed through after 5-10min terminates being passed through for hydrogen again.
Preferably, in step (2), the heating rate of tube furnace is 0.5~1 DEG C/min.
Beneficial effects of the present invention are as follows:
The present invention is asked for reversible capacity is smaller, cycle performance is poor present in current lithium ion battery negative material etc.
Topic introduces sea urchin shape cobaltosic oxide as active material, and deposits one layer of carbon coating on its surface by vapour deposition process.Carbon
Cladding can be overall electrode material with electric, and it is steady to improve structure of the sea urchin shape cobaltosic oxide in charge and discharge process
It is qualitative, so that it is unlikely to that avalanche occurs in rush of current.In addition, in vapor deposition processes under the action of hydrogen, hydrogen meeting
It reacts with the oxygen in cobaltosic oxide, so that the valence state of cobalt changes, the cobalt of mixed valence can be electrode material
Material provides additional electric conductivity.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples:
Fig. 1 is the scanning electron microscope (SEM) photograph that echinus-like carbon obtained by embodiment 1 coats cobalt/cobalt oxide.
Fig. 2 is the electric discharge specific volume that echinus-like carbon obtained by embodiment 1 coats cobalt/cobalt oxide lithium ion battery negative material
Amount circulation figure.
Specific embodiment
Embodiment 1:
(1) sea urchin shape cobaltosic oxide is prepared:
0.3g cobalt chloride is taken, 2g urea is dissolved in 50mL deionized water, and magnetic agitation 2h is transferred to after mixing evenly
It in 150mL reaction kettle, is placed in constant temperature oven, 120 DEG C of reaction 18h, subsequent furnace cooling is respectively washed using deionized water with ethyl alcohol
Three times, 60 DEG C of dryings in baking oven are placed in.It places it in Muffle furnace again after the completion, 300 DEG C of calcining 8h obtain the oxidation of sea urchin shape four
Three cobalts.
(2) echinus-like carbon cladding cobalt/cobalt oxide is prepared:
The sea urchin shape cobaltosic oxide powder 0.2g being prepared in step 1 is placed in tube furnace, under an argon atmosphere
600 DEG C are warming up to the heating rate of 1 DEG C/min, is passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, wherein hydrogen
Gas velocity is 200mL/min, and acetylene flow velocity is 30mL/min, is continually fed into 2min, is first shut off acetylene after the completion, and acetylene is closed
Hydrogen is turned off after 5min, under an argon atmosphere natural cooling, obtain echinus-like carbon cladding cobalt/cobalt oxide.
Embodiment 2:
(1) sea urchin shape cobaltosic oxide is prepared:
0.1g cobalt chloride is taken, 1g urea is dissolved in 10mL deionized water, and magnetic agitation 1h is transferred to after mixing evenly
It in 150mL reaction kettle, is placed in constant temperature oven, 100 DEG C of reaction 12h, subsequent furnace cooling is respectively washed using deionized water with ethyl alcohol
Three times, 60 DEG C of dryings in baking oven are placed in.It places it in Muffle furnace again after the completion, 200 DEG C of calcining 6h obtain the oxidation of sea urchin shape four
Three cobalts.
(2) echinus-like carbon cladding cobalt/cobalt oxide is prepared:
The sea urchin shape cobaltosic oxide powder 0.1g being prepared in step 1 is placed in tube furnace, under an argon atmosphere
500 DEG C are warming up to the heating rate of 0.5 DEG C/min, is passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, wherein
Hydrogen flow rate is 100mL/min, and acetylene flow velocity is 10mL/min, is continually fed into 1min, is first shut off acetylene after the completion, and acetylene closes
Hydrogen is turned off after closing 7min, under an argon atmosphere natural cooling, obtains echinus-like carbon cladding cobalt/cobalt oxide.
Embodiment 3:
(1) sea urchin shape cobaltosic oxide is prepared:
0.5g cobalt chloride is taken, 5g urea is dissolved in 100mL deionized water, and magnetic agitation 3h is transferred to after mixing evenly
It in 150mL reaction kettle, is placed in constant temperature oven, for 24 hours, subsequent furnace cooling is respectively washed using deionized water with ethyl alcohol for 150 DEG C of reactions
Three times, 60 DEG C of dryings in baking oven are placed in.It places it in Muffle furnace again after the completion, 400 DEG C of calcining 12h obtain the oxidation of sea urchin shape four
Three cobalts.
(2) echinus-like carbon cladding cobalt/cobalt oxide is prepared:
The sea urchin shape cobaltosic oxide powder 0.5g being prepared in step 1 is placed in tube furnace, under an argon atmosphere
700 DEG C are warming up to the heating rate of 1 DEG C/min, is passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, wherein hydrogen
Gas velocity is 300mL/min, and acetylene flow velocity is 50mL/min, is continually fed into 3min, is first shut off acetylene after the completion, and acetylene is closed
Hydrogen is turned off after 10min, under an argon atmosphere natural cooling, obtain echinus-like carbon cladding cobalt/cobalt oxide.
Claims (9)
1. a kind of preparation method of height ratio capacity lithium ion battery negative material, which is characterized in that the negative electrode of lithium ion battery
Material is that echinus-like carbon coats cobalt/cobalt oxide composite material, and the preparation method comprises the following steps:
(1) sea urchin shape cobaltosic oxide is prepared:
Cobalt chloride, urea are dissolved in deionized water, after magnetic agitation is uniform by mixed liquor be placed in reaction kettle carry out hydro-thermal it is anti-
It answers, natural cooling after hydro-thermal reaction, product is respectively washed three times using deionized water and ethyl alcohol, product is placed in 60 in baking oven
DEG C drying, desciccate are placed in calcining in Muffle furnace and obtain sea urchin shape cobaltosic oxide;
(2) echinus-like carbon cladding cobalt/cobalt oxide is prepared:
The sea urchin shape cobaltosic oxide powder being prepared in step (1) is placed in tube furnace, is warming up under an argon atmosphere
500~700 DEG C, it is passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, after being continually fed into 1~3min, closes hydrogen
And acetylene, natural cooling, obtains echinus-like carbon cladding cobalt/cobalt oxide composite material under an argon atmosphere.
2. preparation method according to claim 1, which is characterized in that in step (1), cobalt chloride, urea and deionized water
Usage ratio are as follows: (0.1~0.5) g:(1~5) g:(10~100) mL.
3. preparation method according to claim 1, which is characterized in that in step (1), the magnetic agitation time is 1~3h.
4. preparation method according to claim 1 or 2, which is characterized in that in step (1), the temperature of the hydro-thermal reaction
Be 100~150 DEG C, the hydro-thermal reaction time be 12~for 24 hours.
5. preparation method according to claim 1-3, which is characterized in that in step (1), the temperature of the calcining
It is 200~400 DEG C, calcination time 6-12h.
6. preparation method according to claim 1, which is characterized in that in step (2), sea urchin shape cobaltosic oxide powder
Quality is 0.1~0.5g, and hydrogen flow rate is 100~300mL/min, and acetylene flow velocity is 10~50mL/min.
7. preparation method according to claim 1, which is characterized in that in step (2), acetylene persistently leads to hydrogen gas mixture
After entering 1~3min, stopping acetylene first is passed through, and acetylene stopping is passed through after 5-10min terminates being passed through for hydrogen again.
8. preparation method according to claim 1 or 6, which is characterized in that in step (2), the heating rate of tube furnace is
0.5~1 DEG C/min.
9. the lithium ion battery negative material that preparation method according to claim 1-8 is prepared.
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Cited By (3)
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CN110993941A (en) * | 2019-12-11 | 2020-04-10 | 肇庆市华师大光电产业研究院 | Preparation method of hollow spherical carbon-coated iron sulfide composite potassium ion battery negative electrode material |
CN111470546A (en) * | 2020-03-17 | 2020-07-31 | 肇庆市华师大光电产业研究院 | Coating material for functional interlayer of lithium-sulfur battery and preparation method thereof |
WO2021008244A1 (en) * | 2019-07-17 | 2021-01-21 | 肇庆市华师大光电产业研究院 | Lithium ion battery negative electrode material with high specific capacity and preparation method therefor |
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CN111470546A (en) * | 2020-03-17 | 2020-07-31 | 肇庆市华师大光电产业研究院 | Coating material for functional interlayer of lithium-sulfur battery and preparation method thereof |
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