CN206422149U - A kind of carbon core/cupric oxide shell combination electrode for lithium ion battery - Google Patents
A kind of carbon core/cupric oxide shell combination electrode for lithium ion battery Download PDFInfo
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- CN206422149U CN206422149U CN201720062309.2U CN201720062309U CN206422149U CN 206422149 U CN206422149 U CN 206422149U CN 201720062309 U CN201720062309 U CN 201720062309U CN 206422149 U CN206422149 U CN 206422149U
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- lithium ion
- cupric oxide
- combination electrode
- ion battery
- carbon fiber
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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 utility model discloses a kind of carbon core/cupric oxide shell combination electrode for lithium ion battery.The core of the carbon core/cupric oxide shell combination electrode is carbon fiber, and shell is copper oxide lamina；Described copper oxide lamina has the nano whiskers structure and nanometer cavernous structure of array type.The preparation method of the carbon core/cupric oxide shell combination electrode comprises the following steps：（1）The preparation of copper carbon fiber；（2）The sinter molding of copper carbon fiber；（3）It is molded the surface oxidation treatment of copper carbon fiber felt.The utility model carbon core/cupric oxide shell combination electrode improves the charge/discharge capacity of lithium ion battery, improves the chemical properties such as cycle life, coulombic efficiency and the cyclical stability of lithium ion battery.
Description
Technical field
The utility model is related to technical field of lithium ion, and in particular to a kind of carbon core/oxygen for lithium ion battery
Change copper shell combination electrode.
Background technology
Lithium ion battery belongs to the chargeable electrochmical power source of green high-capacity, with voltage is high, energy density is big, cycle performance
The outstanding advantages such as good, the small, memory-less effect of self discharge, in delivery vehicle, portable electric appts, communication back-up source, sky
Between the field such as technology, national defense industry be widely applied.
Carbons material is the negative material being most widely used in current lithium ion battery, with suitable intercalation potential
（0.15 ~ 0.25V）, good conductivity, stable circulation, and also aboundresources, it is cheap, turn into the market mainstream for a long time.But
The theoretical specific capacity of carbons material is relatively low（372mAh·g-1）, can not meet too high demand of the people to the energy, therefore people
In the urgent need to storage lithium performance it is good, the high novel active of theoretical capacity substitutes traditional graphite material and is applied to lithium-ion electric
Pond field, to solve the energy in straitened circumstances situation that supply falls short of demand.Transition metal oxide is because its storage lithium performance is good, theoretical capacity
The advantages of high, preparation is simply, raw material sources are extensive causes the strong interest of numerous researchers at home and abroad.Cupric oxide conduct
Most common transition metal oxide, due to the higher (674mAhg of its theoretical specific capacity-1), to prepare simple, cost more low
Advantage, is gradually applied in lithium ion battery.But the electric conductivity of cupric oxide is poor, therefore pure zirconia copper is lived as negative pole
Property material be applied to lithium ion battery in can inevitably result in cycle life, coulombic efficiency and the stable charge/discharge of battery
Decline.In order to solve this problem, numerous researchers it is main at present by add conductive additive, synthetic composite material and
The methods such as modification activities physical form improve cupric oxide as the combination property of the battery of negative electrode active material.Such as by adding
Plus the conductive material such as electrically conductive graphite, CNT, metal dust improves the electric conductivity of electrode, by synthesizing CuO composite Nanos
The cycle life and reversible capacity of the structures such as line, nanometer rods, nano flower to improve battery etc..These methods are all to a certain degree
On solve CuO poorly conductives and cause the problem of battery performance declines.
In addition, lithium ion battery is during cycle charge-discharge, the embedding and removing process inside active material can not be kept away
The expansion and contraction of active material particle volume can be caused with exempting from, so that the powder phenomenon-tion of electrode material is caused, influence battery
Cycle life.Therefore, Volume Changes of the restricted activity material during embedding and removing are undoubtedly extension battery cycle life,
Improve the effective means of battery combination property.Than if any researcher by being limited in one layer of carbon thin layer of silicon grain surface carbonation
The violent Volume Changes of silicon grain in battery charge and discharge process, so as to improve the cycle life and reversible capacity of battery.Also learn
Person makes silicon grain surface realize metallization by electroless copper method, so as to improve every chemical property of lithium ion battery.
Utility model content
In order to improve CuO as the electric conductivity of electrode during cell negative electrode material, limitation carbons active material is in battery charge and discharge
The change of volume in electric process, so as to improve the electrochemistries such as the reversible capacity of battery, cycle life, stable charge/discharge
Can, the utility model provides a kind of carbon core/cupric oxide shell combination electrode for lithium ion battery.
The utility model is achieved through the following technical solutions.
A kind of carbon core/cupric oxide shell combination electrode for lithium ion battery, the carbon core/cupric oxide shell compound electric
The core of pole is carbon fiber, and shell is copper oxide lamina；Described copper oxide lamina has the acicular texture of array type and poroid
Structure.
Further, described acicular texture and cavernous structure are nano-scale structures.
Further, the acicular texture is in the outer surface of copper oxide lamina, and the cavernous structure is that insertion cupric oxide is thin
The hole of layer.
Further, carbon core/cupric oxide shell combination electrode for lithium ion battery uses a diameter of 14 ~ 15mm, thick
Spend the sintered shaping of copper carbon fiber felt for 0.1 ~ 0.2mm and surface oxidation treatment is formed.
A kind of preparation method of described carbon core/cupric oxide shell combination electrode for lithium ion battery, including copper facing
The preparation of carbon fiber, the sinter molding of copper carbon fiber and the surface oxidation treatment for being molded copper carbon fiber felt.
Further, the preparation of the copper carbon fiber, comprises the following steps：
（1）Desizing：Carbon fiber is placed in calcination in high temperature resistance furnace air, the protection of carbon fiber surface is removed
Glue, improves the adhesion of coating and carbon fiber, reduces the contact resistance between coating and carbon fiber；
（2）Surface coarsening：Carbon fiber after calcination is placed in (NH4)2S2O8Ultrasonic wave soaks in solution, makes carbon fiber surface
Face is roughened and in hydrophily；Then soaked with NaOH solution, remove the remaining (NH of carbon fiber surface4)2S2O8, then use deionization
Water is cleaned；
（3）Surface sensitizing：Carbon fiber after roughening is placed in by SnCl2, HCl and H2Soaked in the sensitizing solution that O is formulated
Bubble, then carries out hydrostatic rinsing with deionized water；
（4）Surface active：Carbon fiber after sensitization is placed in by AgNO3、NH3·H2O and H2The activating solution that O is formulated
Middle immersion, is then cleaned carbon fiber to black with deionized water；
（5）Copper coating：Carbon fiber after activation is placed in by NaKC4H4O6·4H2O、CuSO4·5H2O、HCHO、NaOH
And H2In the plating solution that O is formulated, produced, finally cleaned with deionized water, very with magnetic stirrer to solution bubble-free
Sky drying, obtains the copper carbon fiber.
Further, step（1）In, the length of the carbon fiber is 1 ~ 2mm.
Further, step（1）In, the calcination is 30 ~ 40min of calcination at 400 ~ 500 DEG C.
Further, step（2）In, (the NH4)2S2O8The concentration of solution is 15 ~ 17wt%.
Further, step（2）In, in (NH4)2S2O8The time that ultrasonic wave soaks in solution is 30 ~ 40min.
Further, step（2）In, the concentration of the NaOH solution is 9 ~ 11wt%.
Further, step（2）In, the time soaked in NaOH solution is 5 ~ 10min.
Further, step（2）In, the deionized water cleaning is that cleaning to cleaning solution is in neutrality.
Further, step（3）In, by SnCl2, HCl and H2In the sensitizing solution that O is formulated, SnCl2Concentration be
0.01~0.02g·mL-1, HCl concentration is 38 ~ 40mLL-1。
Further, step（3）In, the time of the immersion is 5 ~ 10min.
Further, step（3）In, the number of times of the hydrostatic rinsing is 3 ~ 4 times.
Further, step（4）In, by AgNO3、NH3·H2O and H2In the activating solution that O is formulated, AgNO3It is dense
Spend for 0.004 ~ 0.005gmL-1、NH3Concentration be 9 ~ 10mLL-1。
Further, step（4）In, the time of the immersion is 5 ~ 10min.
Further, step（5）In, by NaKC4H4O6·4H2O、CuSO4·5H2O, HCHO, NaOH and H2O prepare and
Into plating solution in, NaKC4H4O6Concentration be 0.04 ~ 0.05gmL-1, CuSO4Concentration be 0.01 ~ 0.02gmL-1, HCHO
Concentration be 9 ~ 10mLL-1, NaOH concentration is 0.01 ~ 0.02 gmL-1。
Further, step（5）In, the rotating speed of the magnetic stirrer is 300 ~ 400rmin-1。
Further, step（5）In, the deionized water cleaning is that cleaning to cleaning solution is in neutrality.
Further, step（5）In, the vacuum drying is 5 ~ 6h of baking at 50 ~ 60 DEG C.
Further, the copper carbon fiber sinter molding, comprises the following steps：
Copper carbon fiber is pressed into fibrofelt with mould, is placed in vacuum resistance furnace, high temperature sintering, obtains being molded copper facing
Carbon fiber felt.
Further, a diameter of 14 ~ 15mm of the carbon fiber felt, thickness is 0.1 ~ 0.2mm.
Further, the sintering is to carry out in a hydrogen atmosphere.
Further, the temperature of the sintering is 750 ~ 800 DEG C, and the time of sintering is 60 ~ 70min.
Further, the surface oxidation treatment of the shaping copper carbon fiber felt, comprises the following steps：
Shaping copper carbon fiber felt is placed in Muffle furnace, air atmosphere high temperature heated oxide, obtains described for lithium
The carbon core of ion battery/cupric oxide shell combination electrode.
Further, the temperature of the heated oxide is 400 ~ 450 DEG C, and the time is 1 ~ 2h.
Compared with prior art, the utility model has the following advantages that and beneficial effect：
（1）The utility model is used in carbon core/cupric oxide shell combination electrode of lithium ion battery, and copper oxide lamina is received
Rice cavernous structure is conducive to the lithium ion in electrolyte to easily pass through, and then occurs embedding and removing process in carbon core, so that
Increase the charge/discharge capacity of lithium ion battery；
（2）The utility model is used for the carbon core/cupric oxide shell combination electrode, carbon core segment and cupric oxide of lithium ion battery
Shell is in close contact, and had both improved the electric conductivity of electrode, the Volume Changes degree in cupric oxide conversion process has been buffered again；
（3）The utility model is used for carbon core/cupric oxide shell combination electrode of lithium ion battery, and cupric oxide shell is closely
Carbon core segment is wrapped in, and the nano whiskers structure of cupric oxide shell highly shortened the diffusion length of lithium ion and add
Effective contact area between lithium ion, limits carbon fiber volume during lithium ion battery discharge and recharge embedding and removing
Expansion, so as to be conducive to improving the reversible capacity and cycle life of lithium ion battery.
Brief description of the drawings
Fig. 1 is the overall structure diagram of the carbon core/cupric oxide shell combination electrode prepared in embodiment 1；
Fig. 2 is the partial schematic diagram of the carbon core/cupric oxide shell combination electrode prepared in embodiment 1；
Fig. 3 is the assembling schematic diagram of the lithium ion half-cell equipped with carbon core/cupric oxide shell combination electrode in embodiment 2；
Fig. 4 is the cycle charge discharge electrical measurement of the lithium ion half-cell equipped with carbon core/cupric oxide shell combination electrode in embodiment 2
Try curve map.
Embodiment
To further understand the utility model, the utility model is described further with reference to the accompanying drawings and examples,
It should be understood that, the claimed scope of the utility model is not limited to the scope of embodiment statement, claim
Other unrequited embodiments of wide parameter are equally effective.
Embodiment 1
A kind of preparation of carbon core/cupric oxide shell combination electrode for lithium ion battery, comprises the following steps：
The preparation of copper carbon fiber
（1）Desizing：Length is placed in calcination 30min in high temperature resistance furnace air, calcination temperature for 1mm carbon fiber
Spend for 400 DEG C, to remove the Protection glue of carbon fiber surface, improve the adhesion of coating and carbon fiber, reduce coating and carbon fiber
Between contact resistance；
（2）Surface coarsening：Carbon fiber after removing glue is placed in the (NH that concentration is 15wt%4)2S2O8Ultrasonic wave soaks in solution
30min is steeped, carbon fiber surface is roughened and in hydrophily；The NaOH solution for being then 10wt% with concentration soaks 5min to it, removes
(the NH for going carbon fiber surface remaining4)2S2O8, and carbon fiber is cleaned to cleaning solution in neutrality；
（3）Surface sensitizing：Carbon fiber after roughening is placed in by SnCl2, HCl and H2The sensitizing solution that O is formulated（Sensitization
In liquid, SnCl2Concentration be 0.02gmL-1, HCl concentration is 40mLL-1）Middle immersion 10min, then with deionized water pair
Carbon fiber carries out hydrostatic and rinsed 3 times；
（4）Surface active：Carbon fiber after sensitization is placed in by AgNO3、NH3·H2O and H2The activating solution that O is formulated
（In activating solution, AgNO3Concentration be 0.005gmL-1, NH3·H2O concentration is 10mLL-1）Middle immersion 10min, then
Carbon fiber is cleaned to black with deionized water；
（5）Copper coating：Carbon fiber after activation is placed in by NaKC4H4O6·4H2O、CuSO4·5H2O、HCHO、NaOH
And H2The plating solution that O is formulated（In plating solution, NaKC4H4O6Concentration be 0.04gmL-1, CuSO4Concentration be 0.01gmL-1, HCHO concentration is 10mLL-1, NaOH concentration is 0.01gmL-1）In, with magnetic stirring apparatus with 400rmin-1's
Rotating speed is stirred to solution bubble-free and produced, and it is in neutral finally to be cleaned copper carbon fiber to cleaning solution with deionized water, and vacuum
60 DEG C of drying 6h, obtain copper carbon fiber.
The sinter molding of copper carbon fiber
（6）Compacting：50mg copper carbon fiber is pressed into a diameter of 15mm, thickness is 0.1mm fibrofelt；
（7）Sintering：The fibrofelt of compacting is placed in vacuum resistance furnace, in a hydrogen atmosphere, high temperature sintering, sintering temperature
For 800 DEG C, soaking time is 60min, obtains being molded copper carbon fiber felt.
It is molded the surface oxidation treatment of copper carbon fiber felt
（8）The shaping copper carbon fiber felt of gained is placed in Muffle furnace, in atmosphere high-temperature heating oxidation, heating-up temperature
For 400 DEG C, soaking time is 2h, obtains the carbon core/cupric oxide shell combination electrode for lithium ion battery.
The overall structure diagram and part of the carbon core for the lithium ion battery/cupric oxide shell combination electrode prepared are shown
It is intended to respectively as depicted in figs. 1 and 2, including core and shell, core is carbon fiber 11, and shell is copper oxide lamina；Cupric oxide
Thin layer has the nano whiskers structure 9 and nanometer cavernous structure 10 of array type, appearance of the nano whiskers structure 9 in copper oxide lamina
Face, nanometer cavernous structure 10 is the hole of insertion copper oxide lamina.
Embodiment 2
The assembling schematic diagram of carbon core prepared by embodiment 1/cupric oxide shell combination electrode assembling lithium ion half-cell is such as
Shown in Fig. 3, including upper battery case 1, shell fragment 2, pad 3, lithium piece 4, barrier film 5, electrolyte 6, lower battery case 7 and carbon core/cupric oxide
Shell combination electrode 8；
Carbon core/cupric oxide shell combination electrode 8 is placed on lower battery case 7, and electrolyte 6 is full of by carbon core/cupric oxide shell
Active material is filled with the whole cavity that combination electrode 8, lower battery case 7 and barrier film 5 are constituted, whole cavity, electrolyte 6 is straight
Connect the active material on infiltration carbon core/cupric oxide shell combination electrode 8；Lithium piece 4 is close on barrier film 5, the upper surface of lithium piece 4 by
Under it is supreme be sequentially placed pad 3 and shell fragment 2, pad 3 and shell fragment 2 play a part of adjusting pressure, shell fragment 2 and upper battery case 1
It is in close contact to reduce contact resistance, it is ensured that the good electric conductivity of inside battery.
After the completion of the assembling of lithium ion half-cell, during electric discharge, lithium piece 4 starts de- lithium, and lithium ion enters electrolysis by barrier film 5
In liquid 6, then change with the active contacts on carbon core/cupric oxide shell combination electrode 8, be embodied in lithium from
Son is directly converted by electrolyte with 9, and occurs process of intercalation through nanostructured 10 and then with 11；At the same time, it is electric
It is sub successively to enter lower battery case 7 by pad 3, shell fragment 2 and upper battery case 1, due to lower battery case 7 and carbon core/cupric oxide outside
Shell combination electrode 8 is in close contact, thus electronics enter in the active material of carbon core/cupric oxide shell combination electrode 8 with lithium from
Son carries out charging neutrality, completes the discharge process of lithium ion half-cell；And the charging process of lithium ion half-cell is just opposite.
Described lithium ion half-cell is in charge and discharge process, because the nano whiskers structure of cupric oxide shell greatly contracts
The short diffusion length of lithium ion and effective contact area between lithium ion is added, thus the reversible capacity of battery can be with
It is greatly improved.In addition, the nanometer cavernous structure of cupric oxide is conducive to the lithium ion in electrolyte to easily pass through, Jin Er
Embedding and removing process occurs in carbon core, so as to increase the charge/discharge capacity of battery.During the cycle charge-discharge of battery, carbon
Core segment is in close contact with cupric oxide shell, had both improved the electric conductivity of electrode, the body in cupric oxide conversion process has been buffered again
Product intensity of variation；Cupric oxide shell is closely wrapped in carbon core segment, during limiting embedding and removing to a certain extent
The Volume Changes of carbon core, so as to be conducive to improving the reversible capacity and cycle life of battery.
Cycle charge discharge electrical testing is carried out to the lithium ion half-cell of assembling with LAND battery test systems CT2001A, obtained
Test curve it is as shown in Figure 4.As can be seen that there is carbon core/cupric oxide shell combination electrode from curve（CuO-CF）Lithium from
Sub- battery is than only oxidation copper electrode（CuO）Only carbon fiber electrode（CF）Lithium ion battery have higher reversible capacity
With more preferable high rate performance.Wherein there is the current condition in 0.1C of the lithium ion battery of carbon core/cupric oxide shell combination electrode
Under reversible specific capacity be up to 671.2mAh/g, significantly larger than only oxidation copper electrode and the only lithium-ion electric of carbon fiber electrode
Pond.Under the conditions of different multiplying powers, there is the reversible capacity of lithium ion battery of carbon core/cupric oxide shell combination electrode relative to it
His two kinds of batteries also very advantageous.In addition, after 0.1C, 0.2C, 0.5C, 1C and 2C rate charge-discharge, there is carbon core/cupric oxide
The lithium ion battery of shell combination electrode reversible capacity under 0.1C current condition is still maintained at 637.4 mAh/g, accounts for again
The 94.8% of the stable capacity of battery before rate discharge and recharge, as a result show carbon core/cupric oxide shell combination electrode can effectively improve lithium from
Every chemical property of sub- battery.
Above-described embodiment of the present utility model is only intended to clearly illustrate the utility model example, and is not
Restriction to embodiment of the present utility model.For those of ordinary skill in the field, on the basis of described above
On can also make other changes in different forms.There is no necessity and possibility to exhaust all the enbodiments.
All any modifications, equivalent substitutions and improvements made within spirit of the present utility model and principle etc., should be included in this reality
Within new scope of the claims.
Claims (4)
1. a kind of carbon core/cupric oxide shell combination electrode for lithium ion battery, it is characterised in that the carbon core/cupric oxide
The core of shell combination electrode is carbon fiber, and shell is copper oxide lamina；Described copper oxide lamina has the needle-like of array type
Structure and cavernous structure.
2. a kind of carbon core/cupric oxide shell combination electrode for lithium ion battery according to claim 1, its feature exists
In described acicular texture and cavernous structure is nano-scale structures.
3. a kind of carbon core/cupric oxide shell combination electrode for lithium ion battery according to claim 1, its feature exists
In the acicular texture is in the outer surface of copper oxide lamina, and the cavernous structure is the hole of insertion copper oxide lamina.
4. a kind of carbon core/cupric oxide shell combination electrode for lithium ion battery according to claim 1, its feature exists
In carbon core/cupric oxide shell combination electrode for lithium ion battery uses a diameter of 14 ~ 15mm, and thickness is 0.1 ~ 0.2mm's
The sintered shaping of copper carbon fiber felt and surface oxidation treatment are formed.
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