CN108183213A - A kind of preparation method of di-iron trioxide/carbon/carbon nanotube lithium battery negative material - Google Patents
A kind of preparation method of di-iron trioxide/carbon/carbon nanotube lithium battery negative material Download PDFInfo
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- CN108183213A CN108183213A CN201711445938.4A CN201711445938A CN108183213A CN 108183213 A CN108183213 A CN 108183213A CN 201711445938 A CN201711445938 A CN 201711445938A CN 108183213 A CN108183213 A CN 108183213A
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- H01M4/00—Electrodes
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- 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
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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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- 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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Abstract
The present invention is a kind of preparation method of di-iron trioxide/carbon/carbon nanotube lithium battery negative material, is included the following steps：The first step is added to after mixing carbon nanotube and KOH powder in distilled water, and after stirring, dry, roasting obtains Activated Carbon Nanotubes；Second step, by Fe (NO3)9And C6H12O6Mixed liquor, with will activate after CNT dispersion mix after react, obtain Fe2O3/C/CNT.The shortcomings of present invention combines carbon-coated di-iron trioxide nano particle together with carbon nanotube, and the conductivity occurred when can improve carbon coating di-iron trioxide nano particle as negative electrode of lithium ion battery is low, specific capacity is low and coulombic efficiency is relatively low.
Description
Technical field
The present invention relates to electrode material of lithium battery, more particularly to a kind of Fe with high electrochemical performance2O3/C/CNT
The preparation method of lithium ion battery negative material.
Background technology
With the continuous development of social progress and science and technology, energy crisis gradually becomes puzzlement with environmental pollution
The important problem of mankind's long-term sustainable survival and development.The energy is the material base of human survival, is world economic growth hair
The driving source of exhibition and the important indicator of Civilization development degree.Nowadays, since human society is to the great demand of the energy,
Non-regeneration energy faces exhaustion in nature, and the development and application for causing the energy are encountered by huge challenge.In this context,
It finds extremely urgent with high-energy conversion ratio, reproducible new green power.
New energy includes primary energy and the secondary power supplies such as nuclear energy, solar energy, biomass energy, wind energy, underground heat, ocean energy
In Hydrogen Energy etc..The natural energies such as wind energy, tide energy, solar energy is made full use of to be advantageously implemented the sustainable development tool of human society
There is important strategic importance.However in the large-scale development process of more than natural energy, there are the discontinuous problem of energy effect,
It would therefore be desirable to have matched energy storage devices.Chemical cell is as a kind of most widely used, most convenient, pollution minimum
Chemical energy plays the role of very important and status with electric transformation of energy storage facility in human social development.In recent years, by
Grown rapidly in space and military demand and electronic technology so that it is small, light-weight, safe, service life is long,
Negative environment effects are small, functional, and the big electrochmical power source of energy density becomes the necessity in human kind sustainable development.Tradition
Battery is because low there are energy resource density, the problems such as environmental pollution is serious, and having been unable to meet the growing modern society of the mankind needs
It asks.Lithium rechargeable battery is exactly a kind of novel power supply for meeting current energy development form and rising.Lithium ion battery has
Energy density is high, operating voltage is high, have extended cycle life, charging rate is fast, memory-less effect and the features such as non-environmental-pollution, therefore
It is widely used in the energy storage fields such as electric vehicle, portable electronic device power supply rapidly.
Although the exploitation of lithium ion battery is very ripe, specific capacity has been sufficiently close to the reason of its corresponding material
By specific capacity (300mAh/g), but still can not meet the growing novel battery to environment-friendly type and high-energy-density of people needs
It asks, researching and developing high next-generation energy density, environmental protection and lithium cell cathode material at low cost has become problem to be solved.Fe2O3
Have many advantages, such as that specific capacity is big, nontoxic environmentally friendly and material source high with security performance enriches, cheap oxidation
Iron is a kind of lithium ion battery negative material for having very much development potentiality.But it is led the drawback is that equally having with other transition oxides
The characteristics of electrically poor (2 × 104S/m, 25 DEG C), and have body up to~200% along with the insertion and abjection of lithium ion
Product variation, thus it is its chemical property, cyclical stability, forthright unsatisfactory again.Carbon coating Fe2O3It can effectively be alleviated to fill
The volume expansion occurred in discharge process increases its electric conductivity, Fe2O3/ C is in pomegranate shape core-shell structure, and CNT is with good
Crystallinity thus the superior conductive network of electric conductivity can be formed in the electrodes.If by both (Fe that is combined with each other2O3/ C is compounded in
In carbon nanotube) formed hybridization network structure be then more advantageous to Fe2O3It can improve three while the charge transmission of electrolyte interface
Aoxidize two iron reacted with lithium cause material volume expand caused by stress, can then improve the cyclicity of di-iron trioxide
Energy and high rate performance.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of di-iron trioxide/carbon/carbon nanotube lithium
The preparation method of cell negative electrode material.Be uniformly mixed first with KOH and carbon nanotube, with tube furnace be heat-treated its mixture from
And achieve the effect that activated carbon nano-tube, the Fe with high electrochemical performance is then prepared using hydro-thermal method2O3/ C/CNT lithium ions
Cell negative electrode material.The present invention is by improving the capacity of electrode carbon nanotube and carbon coating di-iron trioxide are compound.
The technical scheme is that：
A kind of preparation method of di-iron trioxide/carbon/carbon nanotube lithium battery negative material, includes the following steps
The first step prepares Activated Carbon Nanotubes
(1) it is added in distilled water, stirs 20-40 minutes after mixing carbon nanotube and KOH powder；Wherein, mass ratio
Carbon nanotube：KOH powder=1:4-6 often adds 4-6gKOH powder in 100mL distilled water；
(2) by air drying of step (1) products therefrom at 100-150 DEG C；
(3) step (2) products therefrom is put into ceramic boat in horizontal pipe furnace and nitrogen is passed through with 240-280ml/min,
850 DEG C are warming up to the speed of 2-5 DEG C/min and keeps the temperature 1-2 hours, cool to room temperature taking-up；Then it is washed to neutrality with distillation；
Again in 100-150 DEG C of air drying 12-20h；Obtain Activated Carbon Nanotubes；
Second step, Fe2O3The preparation of/C/CNT
(1) by Fe (NO3)9And C6H12O6It is added in deionized water, then stirs 30-40min；Wherein, per 80mL go from
Sub- water adds 1.5-4.0gFe (NO3)3·9H2O；Mass ratio Fe (NO3)3·9H2O and C6H12O6=1：0.74-0.78；After activating
CNT dissipate in deionized water, stir 30-40min；Wherein, after adding in 0.16-0.17g activation in deionized water in every 40mL
CNT；
(2) step (2) acquired solution is poured into the solution in step (1), stirs 30-35min, ultrasonic disperse 1-
1.5h；Wherein, the CNT after mass ratio activation：Fe(NO3)3·9H2O=1：5.5-5.6；
(3) step (3) acquired solution is positioned in the inner liner of reaction kettle of polytetrafluoroethylene (PTFE), with 190- in insulating box
200 DEG C of reaction 9-10h；Last Centrifugal dispersion after obtained solid drying, obtains Fe2O3/C/CNT.
Beneficial effect of the present invention is as follows:
(1) in design process of the invention, in order to solve high conductivity in existing lithium cell cathode material, high stability compared with
The problem of poor, proposes hydro-thermal method complex iron oxide and carbon nanotube.Hydro-thermal method has that product purity is high, scattered, granularity is easily controlled
The advantages that processed so that be difficult to dissolve under usual terms or undissolved substance is dissolved and recrystallized.Hydro-thermal reaction generation
Di-iron trioxide is spherical in shape, and between 300~500nm, particle is stacked with or flocks together with particle size, and entire product gathers
Group is more serious, but the Fe prepared using hydro-thermal reaction method2O3/ C/CNT causes the Fe of spherical core-shell structure2O3/ C is attached to carbon and receives
On mitron.So CNT can play the role of disperseing and support di-iron trioxide and be easy to reunite so as to overcome di-iron trioxide
The shortcomings that.
(2) in design process of the invention, the structure problem in lithium cell cathode material has been fully considered.Nanometer three aoxidizes
Two iron provide more embedding lithium positions so embedding lithium capacity is up to 931mAh/g as negative material according to nanostructured.Because
Nano material is reunited during charge and discharge so with the increase of charging times, the width of each loop attenuation of capacity
Degree is stronger.The advantage in structure is lost, causes stable cycle performance reduction.It prevents or prolongs to a certain extent after introducing CNT
Expansion, dusting and reunion that iron oxide occurs in discharge process are delayed, so as to improve the same of the cyclical stability of iron oxide
When play the role of provide point-like electron channel.
Compared with prior art, the marked improvement of the method for the present invention is as follows
CNIO4505498A uses floating catalytic chemical vapour deposition technique compared with prior art, and hydro-thermal method synthesis is simple and fast
And safety, experiment is substantially non-toxic to humans using drug, and security risk during the experiment is also smaller.Floating catalytic
Chemical vapour deposition technique is needed by the use of thiophene as accelerating agent, and thiophene is inflammable, toxic, is absorbed through skin or steam can cause poisoning.
Argon gas need to be changed into when by the use of vertical heater as reactor hidden in the presence of safety while hydrogen increases the requirement to laboratory technician
Suffer from.There is a small amount of substance respectively to suspend in water when the two is combined with each other and do not form composite construction.Have in hydro-thermal method dried
Journey can make the compound diffusion for inhibiting CNT again of two kinds of materials.Compared to di-iron trioxide/carbon nanotube, di-iron trioxide/
Carbon/carbon nanotube can more improve cyclicity, the high rate performance for the shortcomings that di-iron trioxide improving the success rate tested and material.Cause
Also there is good electric conductivity, high stability and flexibility for carbon, if by di-iron trioxide and its it is compound both can profit
With the excellent electric conductivity of graphite come the defects of making up di-iron trioxide electric conductivity, and the body of di-iron trioxide can be inhibited using it
The shortcomings that product bulking effect and inhibition di-iron trioxide are easy to reunite.
Description of the drawings
Fig. 1 is 1 obtained di-iron trioxide of embodiment/carbon nanotube (Fe2O3/ CNT) low power SEM image
Fig. 2 is 1 obtained di-iron trioxide of embodiment/carbon nanotube (Fe2O3/ CNT) XRD spectrum
Fig. 3 is 1 obtained di-iron trioxide of embodiment/carbon nanotube (Fe2O3/ CNT) as ion cathode material lithium
First lap charging and discharging curve figure.
Specific embodiment
Embodiment 1
1. prepare Activated Carbon Nanotubes
(1) with electronic scale weighing 1g carbon nanotubes (CNT) (having purified, grain size 30-50nm) and 4g KOH (ratios 1:4)
It is first put into agate mortar that the two ground and mixed is uniform, then pours into again in 150ml beakers and add in the mixing of 100ml distilled water,
30min is stirred with magnetic agitation instrument；
(2) by step (1) products therefrom using drying box 100 DEG C air drying for 24 hours, by the moisture in mixture
All evaporation obtains dry mixture；
(3) step (2) products therefrom is put into ceramic boat in horizontal pipe furnace and nitrogen is passed through with 240ml/min, with 5
DEG C/speed of min is warming up to 850 DEG C and keeps the temperature 1 hour, room temperature taking-up is cooled to, carbon nanotube is activated by KOH at this time, KOH
In the tube wall of embedded carbon nanotube；
(4) due to the presence of KOH, (3) obtained carbon nanotube is alkaline, so its product is put into centrifuge tube
In, deionized water is added in, is put into centrifuge after shaking uniformly and centrifuges 10min under the rotating speed of 6000r/min, be centrifuged repeatedly 6 times
The carbon nanotube of activation is washed till neutrality；
(5) and then by centrifugation product it is put into thermostatic drying chamber, the dry 12h under 100 DEG C of air atmospheres；
(6) it is collected and ground using mortar, obtain activated carbon nano-tube powder.
2.Fe2O3The preparation of/C/CNT
(1) electronic scale weighs 2.42g Fe (NO3)3, 1.8g C6H12O6.80ml deionized waters are measured with 100ml graduated cylinders,
It is uniformly mixed after being mixed in beaker with magnetic agitation instrument stirring 30min；
(2) CNT after activation is dissipated with beaker after weighing 40ml deionized waters with graduated cylinder and uses magnetic in 40ml deionized waters
Power stirring instrument stirring 30min；
(3) stirring 30min in step (1) will be poured into obtained by step (2), recycles ultrasonic machine ultrasonic disperse 1h；
(4) it will be positioned in the inner liner of reaction kettle of polytetrafluoroethylene (PTFE) obtained by step (3), with 190 DEG C of reactions in insulating box
9h；
(5) (4) products therefrom is poured into centrifuge tube, adds in deionized water, be put into centrifuge after shaking uniformly
10min is centrifuged under the rotating speed of 6000r/min, is centrifuged repeatedly 6 times, then outwells supernatant liquor, obtains Fe2O3/ C/CNT, is put
Enter in thermostatic drying chamber, dry 12 under the conditions of 60 DEG C；
(6) (5) products therefrom with agate mortar is ground and collected, obtain powdered Fe2O3/C/CNT。
3. electrochemical property test
Fe is tested at room temperature (25 ± 1) DEG C2O3The chemical property of/C/CNT electrodes, by the Fe of preparation2O3/ C/CNT powder
8 are pressed with PVDF and BC:1:1 mass ratio is uniformly mixed in N-Methyl pyrrolidone (NMP) solution, and grinding is after a certain period of time
The suitable slurry of viscosity is configured to, and is coated uniformly on Cu foils, after 60 DEG C are dried in vacuo 4h, cut-parts obtain cathode
Pole piece.Electrochemical property test uses button cell, and metal lithium sheet is used as to electrode, and lithium ion battery is applicable in electrolyte, is used
Polypropylene screen is as diaphragm.Battery pack is mounted in the glove box full of argon gas and carries out.It is mostly logical using the new prestige public affairs CT-4008 types in Shenzhen
Road cell tester is in laboratory to Fe under constant temperature (25 DEG C)2O3/ C/CNT nano composite anode materials are tested.
Embodiment 2
Other prepare Fe with embodiment 1, difference for second step2O3(4) step in/CNT materials is positioned over polytetrafluoro
In the inner liner of reaction kettle of ethylene, with 210 DEG C of reaction 9h in insulating box.
Embodiment 3
Other prepare Fe with embodiment 1, difference for second step2O3(4) step in/CNT materials is positioned over polytetrafluoro
In the inner liner of reaction kettle of ethylene, with 230 DEG C of reaction 9h in insulating box.
Fig. 1 is 1 obtained di-iron trioxide/carbon/carbon nanotube (Fe of embodiment2O3/ CNT) low power SEM image.From
It can be found that successfully having synthesized Fe by hydro-thermal method in XRD diagram2O3With the composite material of carbon nanotube
Fig. 2 is 1 obtained di-iron trioxide/carbon/carbon nanotube (Fe of embodiment2O3/ C/CNT) XRD diagram.Scheme from SEM
In as can be seen that carbon-coated di-iron trioxide bead is uniformly adhered to the surface of carbon nanotube, this illustrates us successfully
The di-iron trioxide bead of shell core shape is successfully compounded in the surface of carbon nanotube, the conduction that this composite material has had
Rate, coulombic efficiency and higher capacity.
This illustrates that the present invention is not carbon nanotube and carbon coating di-iron trioxide is simply compound, but successfully handle
Carbon coating ferric oxide particle is attached to the tube wall of carbon nanotube.The present invention carbon-coated di-iron trioxide nano particle and
Carbon nanotube combines together, occurs when can improve carbon coating di-iron trioxide nano particle as negative electrode of lithium ion battery
Conductivity is low, the shortcomings of specific capacity is low and coulombic efficiency is relatively low.
Fig. 3 is 1 obtained di-iron trioxide/carbon/carbon nanotube (Fe of embodiment2O3/ C/CNT) as lithium-ion negative pole
The first lap charging and discharging curve figure of material.From charge and discharge electrograph it can be found that Fe2O3/C/CNT is as negative electrode of lithium ion battery material
Material, very high specific capacity is showed in the charge and discharge of first lap, reaches 920mAh/g.
Its test condition is：The assembling of button cell：Button cell is assembled in full of argon gas, and humidity is less than 4% hand
It is carried out in casing.According to anode cover, electrode slice, diaphragm, electrolyte, metal lithium sheet, gasket, spring leaf, negative electrode casing sequence according to
Secondary progress.After being completed, assembled button cell is pressed and sealed using tablet press machine.Wherein, diaphragm Celgard
2300 films, electrolyte are the LiPF of 1mol/L6Ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (EMC)
Mixed system (volume ratio 1:1:1), button cell shell model CR2025.Battery case, gasket and spring leaf are before the use
Respectively with deionized water and soaked in absolute ethyl alcohol, it is cleaned by ultrasonic, is put into after being completely dried spare in glove box.The electricity that will be installed
Pond stand 12h after the new prestige public affairs CT-4008 types multi-channel battery test instrument in Shenzhen in laboratory under constant temperature (25 DEG C) it is right
Fe3O4/ C/CNT nano composite anode materials are tested.Constant current loop test current density is 100mA/g, and cycle-index is
200 times.
Unaccomplished matter of the present invention is known technology.
Claims (1)
1. a kind of preparation method of di-iron trioxide/carbon/carbon nanotube lithium battery negative material, it is characterized in that this method packet
Include following steps：
The first step prepares Activated Carbon Nanotubes
（1）It is added in distilled water, stirs 20-40 minutes after carbon nanotube and KOH powder are mixed；Wherein, quality is received than carbon
Mitron：KOH powder=1:4-6 often adds 4-6gKOH powder in 100mL distilled water；
（2）By step（1）Air drying of the products therefrom at 100-150 DEG C；
（3）By step（2）Products therefrom is put into horizontal pipe furnace with ceramic boat and is passed through nitrogen with 240-280ml/min, with 2-5
DEG C/speed of min is warming up to 850 DEG C and keeps the temperature 1-2 hour, it cools to room temperature and takes out；Then it is washed to neutrality with distillation；Exist again
100-150 DEG C of air drying 12-20h；Obtain Activated Carbon Nanotubes；
Second step, Fe2O3The preparation of/C/CNT
（1）By Fe（NO3）9And C6H12O6It is added in deionized water, then stirs 30-40min；Wherein, per 80mL deionized waters
Add 1.5-4.0g Fe（NO3）3·9H2O；Mass ratio Fe（NO3）3·9H2O and C6H12O6=1：0.74-0.78；After activation
CNT is dissipated in deionized water, stirs 30-40min；Wherein, after adding in 0.16-0.17g activation in deionized water in every 40mL
CNT；
（2）By step（2）Acquired solution pours into step（1）In solution in, stir 30-35min, ultrasonic disperse 1-1.5h；Its
In, the CNT after mass ratio activation：Fe（NO3）3·9H2O =1：5.5-5.6；
（3）By step（3）Acquired solution is positioned in the inner liner of reaction kettle of polytetrafluoroethylene (PTFE), with 190-200 DEG C in insulating box
React 9-10h；Last Centrifugal dispersion after obtained solid drying, obtains Fe2O3/C/CNT。
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| CN110690425A (en) * | 2019-09-29 | 2020-01-14 | 上海应用技术大学 | Boron-doped reduced carbon nanotube-loaded ferric oxide composite material and preparation method thereof |
| CN112736235A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Biomass/carbon nanotube induced Fe3O4Nano composite material and application thereof as negative electrode material of lithium ion battery |
| CN112786869A (en) * | 2021-02-09 | 2021-05-11 | 四川轻化工大学 | Preparation method of ferric oxide/spiral carbon nanofiber composite anode material |
| CN113735178A (en) * | 2021-09-06 | 2021-12-03 | 派尔森环保科技有限公司 | Preparation method of lithium ion battery cathode material with iron oxide particles embedded in carbon nitride sheet |
| CN113793931A (en) * | 2021-11-18 | 2021-12-14 | 河南电池研究院有限公司 | Iron oxide negative electrode material for lithium ion battery and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110690425A (en) * | 2019-09-29 | 2020-01-14 | 上海应用技术大学 | Boron-doped reduced carbon nanotube-loaded ferric oxide composite material and preparation method thereof |
| CN112736235A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Biomass/carbon nanotube induced Fe3O4Nano composite material and application thereof as negative electrode material of lithium ion battery |
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| CN112786869B (en) * | 2021-02-09 | 2022-04-01 | 四川轻化工大学 | Preparation method of ferric oxide/spiral carbon nanofiber composite anode material |
| CN113735178A (en) * | 2021-09-06 | 2021-12-03 | 派尔森环保科技有限公司 | Preparation method of lithium ion battery cathode material with iron oxide particles embedded in carbon nitride sheet |
| CN113793931A (en) * | 2021-11-18 | 2021-12-14 | 河南电池研究院有限公司 | Iron oxide negative electrode material for lithium ion battery and preparation method thereof |
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