CN107742699A - Negative electrode of lithium ion battery CuO@beta cyclodextrins core-shell materials and preparation method - Google Patents
Negative electrode of lithium ion battery CuO@beta cyclodextrins core-shell materials and preparation method Download PDFInfo
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- CN107742699A CN107742699A CN201710819672.9A CN201710819672A CN107742699A CN 107742699 A CN107742699 A CN 107742699A CN 201710819672 A CN201710819672 A CN 201710819672A CN 107742699 A CN107742699 A CN 107742699A
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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
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- 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
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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Abstract
The present invention proposes that organic polymer beta cyclodextrin is coated on into the preparation method that CuO surface prepares core shell structure CuO@β CD composites and its composite by paddling process.Compared to the naked materials of CuO, the β CD shells with caking property are coated on CuO kernels, can be alleviated the stress that CuO kernels during repeated charge-discharge cycles are subject to and be played buffer protection function.Other β CD have bonding characteristic, and enhancing the cementitiousness between CuO particulates reduces the loss of active material during charge and discharge cycles.So for cupric oxide as lithium ion battery negative material 50 enclose charge and discharge cycles after capacity attenuation it is more serious the problem of, β CD are coated on the naked material surfaces of CuO with paddling process and are prepared with core shell structure CuO@β CD composites by proposition of the present invention, can effectively lift cyclical stabilities of the CuO as lithium ion battery negative material during repeated charge-discharge cycles.It can be seen in the drawings that the capacity that gained CuO@β CD composites are prepared after the circle of constant current charge-discharge circulation 100 is more than 440 mAh g‑1。
Description
Technical field
The present invention is related to the preparation two of lithium ion battery and transition metal oxide@organic polymer composite materials
Technical field.Mainly beta-schardinger dextrin（β-CD）Coat cupric oxide and prepare CuO@β-CD composites and preparation method, β-CD bags
Gained composite is prepared after covering as lithium ion battery negative material, can compared with without the naked materials of the CuO of any modification
To lift the cyclical stability of lithium ion battery during charge and discharge cycles.
Background technology
Lithium ion battery has that energy density is high, output voltage is high, have extended cycle life, self discharge is few, light weight, memoryless
The advantages that effect, it is widely used to the key areas such as portable electric appts, energy traffic, Aero-Space.Exploitation has height
Energy density, high safety performance, high circulation performance, the lithium ion battery of low cost have turned into field of energy source power at this stage and ground
Study carefully one of focus.The development that lithium ion battery carries out industrialization in field of energy source power is largely dependent upon lifting battery material
The performance of material, wherein negative material are an important factor for influenceing battery energy density height and cyclical stability size.Commercialization
Graphite material because specific capacity it is relatively low（372 mAh g−1）It can not meet people with existing security hidden trouble during use
To the demand of high energy density cells component.2000, French Tarascon seminars delivered related report on Nature
Road, it is indicated that nano transition metal oxides MO（M=Co, Ni, Cu, Fe etc.）Have as lithium ion battery negative material higher
Specific capacity（> 600 mAh g-1）, and the storage lithium mechanism of such material is different from the conventional graphite material of deintercalation formula also different from conjunction
The tinbase and silica-base material of aurification.Transition metal oxide negative material is by carrying out oxygen with lithium metal in charge and discharge process
Change reduction reaction store up lithium, theoretical specific capacity is high, and resource reserve enriches, and easy processing, low cost is lithium ion of new generation
One of candidate of cell negative electrode material, there is preferable development prospect.
Although transition metal oxide has larger specific capacity as lithium ion battery negative material, its stable circulation
Property is poor.The reason for wherein specific capacity is big first mainly has at 2 points：First, electrode surface can be because of electrolyte in discharge process first
Decomposition generate one layer of solid electrolyte（SEI）Passivating film, the generation of SEI films, which can irreversibly consume substantial amounts of Li, causes battery first
Secondary specific capacity is larger；Second, SEI films also can be by the Cu catalytic decomposition consumption part with electro catalytic activity during initial charge
Cu, and Cu and Li during this2O will not react generation CuO completely and reach reversible effect and also result in battery in charge and discharge first
Capacity deep fades in electric process.In addition, the cyclical stability difference of material can be attributed at 2 points：First, CuO is partly led as typical case
The transition metal oxide of body has poor electrical conductivity, and this conduction property can increase polarization of the electrode in electrochemical process
Phenomenon further results in material capacity decay；Second, electrode material can occur due to the effect volume of stress in charge and discharge process
Expansion, material after expansion can further efflorescence cause between material, lose electrical contact between material and collector, and discharged
Agglomeration may also occurs in the nanoscale Cu generated in journey, and the volumetric expansion and reunion of material can all reduce participation reaction
The amount of active material is so as to reducing the cyclical stability of battery.These are all transition metal oxides as negative electrode of lithium ion battery
Material（Including CuO materials）In research the problem of urgent need to resolve.Cladding is carried out to metal oxide and prepares the compound of core shell structure
Material, it can effectively alleviate the stress variation of lithium ion shell during deintercalation, suppress the efflorescence of material, prevent active material and electricity
Solution liquid is reacted, and improves the reversible capacity and cyclical stability of material.
We study cupric oxide as being found after negative electrode of lithium ion battery, and battery is proceeding by constant current charge-discharge circulation
During be demonstrated by higher specific discharge capacity and preferable cyclical stability, but with the continuation of charge and discharge cycles, battery is then
There is more obvious capacity attenuation phenomenon.At present, transition metal oxide material is modified to improve it as negative
The electric conductivity of pole material, suppress efflorescence, reducing the Main Means of reunion and then enhancing chemical property includes：Composite, spy
Different pattern control, material nano and material film.So it is proposed that outside copper oxide material Surface coating beta-schardinger dextrin
Shell prepares the CuO@β-CD composites with core shell structure, and experimental data confirms that the cladding of beta-schardinger dextrin enhances oxygen really
Change cyclical stability of the copper as lithium ion battery negative material in charge and discharge process.Though do not reported in similar way document
Road mistake, but Xue Qi seminars of Nanjing University propose by the use of sulfonated β-cyclodextrin as dopant to be prepared for polypyrrole, in experiment by
The copline of strand is added in the cavity of polypyrrole strand into sulfonated β-cyclodextrin, enhances the electrical conductivity of polypyrrole
And heat endurance.Dopant of East China University of Science Lee et al. using beta-schardinger dextrin as polyaniline, is prepared for self-dispersed conduction
Polyaniline material.Electrically conductive polyaniline, this method effectively carry Zhao Jing the moons seminar of Northwest University using beta-schardinger dextrin as templated synthesis
The high conductance and heat endurance of polymer.
This is applied for a patent using cupric oxide as research object, the shortcomings that for its cyclical stability difference, is stirred by solution
Method prepares CuO@β-CD composites in one layer of beta-schardinger dextrin of copper oxide material Surface coating, and this modified method enhances cupric oxide
Cyclical stability as lithium ion battery negative material.Cladding in this preparation process we have studied β-CD to cupric oxide
CuO@β-CD composites are prepared in the influence of amount, paddling process, realize lifting cupric oxide as negative electrode of lithium ion battery material
Expect the target of cyclical stability.
The content of the invention
The purpose of the present invention one be to provide a kind of used as negative electrode of Li-ion battery beta-schardinger dextrin cladding cupric oxide prepare CuO@β-
CD composites；Another object is to provide the preparation method of the material.
Technical program of the present invention lies in the process in copper oxide material outer cladding beta-schardinger dextrin.On copper oxide material surface
The preparation process for coating beta-schardinger dextrin is as follows：
A certain amount of copper oxide material is weighed in beaker, deionized water is added and stirs, controlling reaction temperature is constant 15
Between~35 °C, weigh beta-schardinger dextrin and add in above-mentioned solution, beta-schardinger dextrin is entered in CuO surface by solution stirring method
The processing of row cladding, continues stirring 2~15 days（d）The composite of beta-schardinger dextrin cladding cupric oxide is prepared.By resulting materials
It is centrifuged and carrying out washing treatment is repeated with deionized water and absolute ethyl alcohol, 60 °C of vacuum drying can obtain CuO
β-CD composites.
Compared to the naked materials of CuO, the CuO@β-CD composites being prepared by paddling process be used to be used as lithium from
Sub- cell negative electrode material, when the β-CD shells with caking property are coated on CuO kernels, to it in charge and discharge process repeatedly
In the stress that is subject to serve the protective effect of buffering, and β-CD bonding characteristic enhances the bonding between CuO particulates
Ability is so as to reducing the loss of active material.Prepared so organic polymer β-CD are coated on into CuO surfaces by paddling process
Obtaining, there is the CuO@β-CD composites of core shell structure can effectively lift CuO is filling repeatedly as lithium ion battery negative material
Cyclical stability in discharge process.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the CuO@β-CD composites obtained by the embodiment of the present invention 1.
Fig. 2 is the energy spectrum diagram of the CuO@β-CD composites obtained by the embodiment of the present invention 1.
Fig. 3 be the embodiment of the present invention 2 obtained by CuO@β-CD composites energy spectrum diagram.
Fig. 4 is CuO@β-CD composites the filling as lithium ion battery negative material obtained by the embodiment of the present invention 2
The charge and discharge cycles curve map of discharge cycles curve map and pure CuO.
Fig. 5 is CuO@β-CD composites the filling as lithium ion battery negative material obtained by the embodiment of the present invention 3
The charge and discharge cycles curve map of discharge cycles curve map and pure CuO.
Fig. 6 is that description of the invention accompanying drawing is made a summary the gained charge and discharge cycles curve map of CuO and CuO@β-CD composites and right
Answer the scanning electron microscope (SEM) photograph of CuO@β-CD composites.
Embodiment
With reference to specific embodiment, the present invention will be further explained.But these embodiments are only used for into one
Step illustrate the present invention, and and be not in any way limit the scope of the present invention.
Embodiment 1：
The preparation of 1.CuO@β-CD composites：
0.4 g black CuO powder is weighed in beaker with 20 mL deionized water dissolvings, is added after the min of magnetic agitation 30
0.8513 g beta-schardinger dextrins.Magnetic agitation 3d and keep reaction system to be constantly in temperature constant state to can obtain CuO β-CD compound
Material.
The purifying of 2.CuO@β-CD composites：
By the CuO@β-CD composites prepared at 4000 turns per minute（rpm）Under conditions of centrifuge three times, 5 minutes every time,
Alternately washing is carried out with deionized water and absolute ethyl alcohol, removes the things such as beta-schardinger dextrin remaining in unreacted ion and system
Matter, finally by CuO@β-CD composites in 60 DEG C of vacuum drying, or freeze-drying.
As shown in the figure：Fig. 1 is the scanning electron microscope image of the CuO@β-CD composites prepared in the present embodiment.Fig. 2 is this
The energy spectrum diagram of CuO@β-CD composites prepared by embodiment.C element peak can see beta-schardinger dextrin composition from the power spectrum
In the presence of.This method has the characteristics of simple, flexible, required production equipment is simple it can be seen from method made above.
Cupric oxide in embodiment 1：The ratio between amount of material of beta-schardinger dextrin is 10:1.5.
Embodiment 2：
0.4 g black CuO powder is weighed in beaker with 20 mL deionized water dissolvings, is added after the min of magnetic agitation 30
0.5675 g beta-schardinger dextrins.Magnetic agitation 3d and keep reaction system to be constantly in temperature constant state to can obtain CuO β-CD compound
Material.
As shown in the figure：Fig. 3 is the scanning electron microscope image that gained CuO@β-CD composites are prepared in the present embodiment.Fig. 4 is
The charge and discharge cycles curve map and pure CuO of CuO@β-CD composites as lithium ion battery negative material in the present embodiment
Charge and discharge cycles curve map.It can be seen that by contrast, core shell structure CuO@β-CD composite woods be prepared by β-CD cladding
When material is used as negative electrode of lithium ion battery, cyclical stability is significantly improved.
Cupric oxide in embodiment 2：The ratio between amount of material of beta-schardinger dextrin is 10:1.
Embodiment 3：
0.4 g black CuO powder is weighed in beaker with 20 mL deionized water dissolvings, is added after the min of magnetic agitation 30
0.2838 g beta-schardinger dextrins.The d of magnetic agitation 3 and keep reaction system to be constantly in temperature constant state to can obtain CuO β-CD multiple
Condensation material.
As shown in the figure：Fig. 5 is the CuO@β-CD composites prepared in the present embodiment as lithium ion battery negative material
Charge and discharge cycles curve map and pure CuO charge and discharge cycles curve map.It can be seen that by contrast, pass through β-CD cladding system
For when obtaining the CuO@β-CD composites of core shell structure as negative electrode of lithium ion battery, cyclical stability is significantly improved.
Cupric oxide in embodiment 3：The ratio between amount of material of beta-schardinger dextrin is 10:0.5.
Embodiment 4：
0.4 g black CuO powder is weighed in beaker with 20 mL deionized water dissolvings, is added after the min of magnetic agitation 30
0.1419 g beta-schardinger dextrins.The d of magnetic agitation 3 and keep reaction system to be constantly in temperature constant state to can obtain CuO β-CD multiple
Condensation material.
Cupric oxide in embodiment 4：The ratio between amount of material of beta-schardinger dextrin is 10:0.25.
Embodiment 5：
0.4 g black CuO powder is weighed in beaker with 20 mL deionized water dissolvings, is added after the min of magnetic agitation 30
0.0142 g beta-schardinger dextrins.The d of magnetic agitation 3 and keep reaction system to be constantly in temperature constant state to can obtain CuO β-CD multiple
Condensation material.
Cupric oxide in embodiment 5：The ratio between amount of material of beta-schardinger dextrin is 10:0.025.
Above-described embodiment is described in detail：By adding beta-schardinger dextrin in this method, by chemical paddling process in cupric oxide
Material surface carries out cladding and CuO@β-CD composites is prepared.CuO@β-CD composites prepared by the present invention are in conduct
In the application of negative electrode of lithium ion battery, there is preferable charge and discharge cycles stability.Prepare beta-schardinger dextrin cladding copper oxide material
Suitable condition be cupric oxide：The ratio between amount of material of beta-schardinger dextrin is 10:0.5~1.5.
Claims (3)
1. organic polymer beta-schardinger dextrin coats cupric oxide, the preparation method of core shell structure CuO@β-CD composites is prepared.Should
The preparation process of composite is as follows：Quantitative black CuO powder is weighed in beaker and with 20 mL deionized water dissolvings and added
With magnetic agitation, quantitative beta-schardinger dextrin powder is added in a period of time backward beaker, keeps whole reaction system to be constantly in perseverance
Warm magnetic agitation state, target product CuO@β-CD composites can be prepared after 2~15 days.
2. the preparation process of the CuO@β-CD composites, its primary focus are described in claims 1：Prepare requisite oxygen
Changing the ratio between amount of material of two kinds of raw materials of copper and beta-schardinger dextrin should control 10:0.5~1.5.
3. follow the preparation process in claims 1, control in claims 2 in composite material is prepared
Experiment parameter, prepare target product CuO@β-CD composites.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710819672.9A CN107742699A (en) | 2017-09-13 | 2017-09-13 | Negative electrode of lithium ion battery CuO@beta cyclodextrins core-shell materials and preparation method |
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| CN201710819672.9A CN107742699A (en) | 2017-09-13 | 2017-09-13 | Negative electrode of lithium ion battery CuO@beta cyclodextrins core-shell materials and preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110707324A (en) * | 2019-10-13 | 2020-01-17 | 浙江大学 | Preparation of conductive adhesive and application of conductive adhesive in battery electrode |
| CN111500105A (en) * | 2020-04-29 | 2020-08-07 | 青岛盈海涂料科技有限责任公司 | Antifouling paint additive and preparation method thereof |
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| CN102074704A (en) * | 2010-12-22 | 2011-05-25 | 上海交通大学 | Preparation method of secondary lithium-sulfur battery anode adhesive |
| CN106698499A (en) * | 2017-01-20 | 2017-05-24 | 江苏先丰纳米材料科技有限公司 | Nano-spherical chain structure copper oxide and preparation method thereof |
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2017
- 2017-09-13 CN CN201710819672.9A patent/CN107742699A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102074704A (en) * | 2010-12-22 | 2011-05-25 | 上海交通大学 | Preparation method of secondary lithium-sulfur battery anode adhesive |
| CN106698499A (en) * | 2017-01-20 | 2017-05-24 | 江苏先丰纳米材料科技有限公司 | Nano-spherical chain structure copper oxide and preparation method thereof |
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| PENGFEI ZONG等: ""Synthesis of Fe3O4/CD magnetic nanocomposite via low temperature plasma technique with high enrichment of Ni(II) from aqueous solution"", 《JOURNAL OF THE TAIWAN INSTITUTE OF CHEMICAL ENGINEERS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110707324A (en) * | 2019-10-13 | 2020-01-17 | 浙江大学 | Preparation of conductive adhesive and application of conductive adhesive in battery electrode |
| CN111500105A (en) * | 2020-04-29 | 2020-08-07 | 青岛盈海涂料科技有限责任公司 | Antifouling paint additive and preparation method thereof |
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Application publication date: 20180227 |