CN109742327A - Preparation method of self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4 positive electrode material - Google Patents
Preparation method of self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4 positive electrode material Download PDFInfo
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- CN109742327A CN109742327A CN201811635476.7A CN201811635476A CN109742327A CN 109742327 A CN109742327 A CN 109742327A CN 201811635476 A CN201811635476 A CN 201811635476A CN 109742327 A CN109742327 A CN 109742327A
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- lifepo
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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 self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4The preparation method of the anode material comprises the steps of preparing LiFePO from citric acid monohydrate, lithium nitrate, ferrous sulfate heptahydrate and ammonium dihydrogen phosphate according to a certain proportion4Adding a three-dimensional carbon cloth material into the precursor sol for soaking, evaporating the solvent while stirring, taking out the carbon cloth at different stages in the sol-gel conversion process, and drying to obtain LiFePO with different loading amounts4The gelled carbon cloth composite material is sintered at high temperature, washed and dried by ultrasonic waves to obtain the composite materialTo the final self-supporting flexible lithium ion battery carbon cloth load LiFePO4A positive electrode material; compared with the traditional coating and sizing process, the composite material prepared by the method has the advantages that the active substances are not easy to fall off, the good flexible effect is achieved, the preparation method is simple, the process period is short, the environment is friendly, no pollution is caused, and the method is suitable for large-scale production.
Description
Technical field
The invention belongs to field of lithium ion battery anode, and in particular to a kind of flexibility lithium ion battery LiFePO4/ carbon
Cloth method for preparing anode material.
Background technique
Lithium ion battery has a high-energy density as a kind of important electrochemical energy storing device, long-time cycle life,
Many advantages, such as reliable safety, has been widely used in the every field of electronics technology, such as portable mobile apparatus, electricity
Electrical automobile etc..However, increasingly sharpening with battery diversified demand, the lithium ion battery device of flexibility, functionalization is met the tendency of
And give birth to, traditional lithium ion cell electrode technology of preparing can no longer meet the demand of cell flexible.Traditional electrode prepares work
Active material and conductive agent, the mixed slurry of binder are coated in metal collector by skill using the method for coating starching.
This structure (is such as stretched, is bent, torsion) in the case where bearing mechanical loading, and active material takes off easily from collector
It falls, causes capacitance loss and the failure of battery.In order to solve the problems, such as electrode flexibility, many researchers use hydro-thermal, CVD method
Active material is grown on flexible current-collecting body (such as nickel foam, carbon paper, carbon cloth, carbon nano-tube film etc.), is constructed " integration "
Electrode, so that effective etc. solve the problems, such as that active material falls off.
Although hydro-thermal, CVD method can well solve the problem of electrode flexibility, the energy density of pole piece and traditional pole
Piece is compared there is also larger gap, and tracing it to its cause be the active material that growth method obtains is nano-scale particle, and load capacity is lower,
Limit the promotion of capacity.Therefore, seek a kind of low cost, efficiently improve the method tool of flexible electrode active material load capacity
It is of great importance.
Summary of the invention
In order to overcome the above-mentioned problems of the prior art, the object of the present invention is to provide a kind of self-supporting flexibility lithiums
Ion battery carbon cloth loads LiFePO4The preparation method of positive electrode chooses LiFePO4As active material, carbon cloth is as flexible
Collector improves flexible electrode energy density by sol-gal process Effective Regulation active material load capacity.
In order to achieve the above object, the present invention adopts the following technical scheme:
A kind of self-supporting flexible lithium ion battery carbon cloth load LiFePO4The preparation method of positive electrode, including following step
It is rapid:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in shape in deionized water
Resulting mixture, wherein monohydrate potassium, lithium nitrate, green vitriol, ammonium dihydrogen phosphate account for the concentration difference of mixture
For 0.2-1mol/L, 0.1-0.5mol/L, 0.1-0.5mol/L and 0.1-0.5mol/L, it is heated to 60 DEG C -80 DEG C and stirs shape
At colloidal sol；
2) carbon cloth is impregnated in above-mentioned colloidal sol, continue to be heated to 60 DEG C -80 DEG C and stirs evaporation solvent；
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out in the process different moments and absorbs gel
Carbon cloth obtains different loads amount LiFePO4The carbon cloth composite material of gel, and be dried, the condition that is dried is 60
It is dry under DEG C -100 DEG C of air atmospheres；
4) by the treated carbon cloth high temperature sintering under an inert atmosphere for absorbing gel, after washed, ultrasound is done
Dry processing obtains final product carbon cloth load LiFePO4Positive electrode, wherein high temperature sintering condition are as follows: be warming up to 600 DEG C -900
6-15h, rear natural cooling are sintered at DEG C.
The foundation that different moments take out carbon cloth in the step 3) is that colloidal sol is evaporated to 1/2,1/4, the 1/ of original volume respectively
10,1/20 when take out carbon cloth.
Inert atmosphere is Ar gas atmosphere in the step 4).
Heating rate is 5 DEG C/min in step 4) the high temperature sintering condition.
Wash conditions are in the step 4): respectively being washed 3 times with deionized water and ethyl alcohol respectively.
Compared with existing technology of preparing, the present invention has following advantageous effects:
Traditional such as CVD method, hydro-thermal method etc., growth activity substance on a flexible substrate, load capacity is often very low, and anti-
It answers process uncontrollable, therefore the energy density of battery pole piece cannot be effectively improved.And the present invention uses sol-gal process in carbon
Carrying active substance in cloth substrate, not only consersion unit is simple, at low cost, and low temperature environment is pollution-free, and in solution from colloidal sol
During gel conversion, Effective Regulation active material load capacity can be reached by simple " dipping-taking-up " method
Purpose, provide reliable method to meet the battery pole piece of different demands, and pass through Experimental comparison and find, different loads
The LiFePO of amount4Carbon cloth surfaces are firmly attached to, the demand of flexibility has been reached, under the conditions of ultimate load and together
LiFePO4Flexible pole piece system comparison, area specific capacity are improved significantly.
Detailed description of the invention
Fig. 1 is pure LiFePO prepared by present example 14(pristine LFP) sample and carbon cloth load LiFePO4
(LFP-CC) the XRD comparison diagram of flexible positive electrode.
Fig. 2 is that carbon cloth prepared by present example 1 loads LiFePO4The SEM of flexible positive electrode schemes, wherein Fig. 2 a is
Scale is 1 μm of obtained SEM shape appearance figure, and Fig. 2 b is that scale is the SEM shape appearance figure that 200nm is obtained.
Fig. 3 is that carbon cloth prepared by present example 3 loads LiFePO4The SEM of flexible positive electrode schemes.
Specific embodiment
Below in conjunction with attached drawing and embodiment, the present invention is described in further detail.
Embodiment 1
A kind of self-supporting flexible lithium ion battery carbon cloth of the present embodiment loads LiFePO4The preparation method of positive electrode, packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in deionized water, respectively
Concentration of component is respectively 0.2mol/L, 0.1mol/L, 0.1mol/L and 0.1mol/L, and aqueous solution whole volume is 20mL, and 80 DEG C
Heating stirring forms colloidal sol.
2) carbon cloth is impregnated in above-mentioned colloidal sol, continues 80 DEG C of heating stirring evaporation solvents.
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out when colloidal sol is evaporated to 10mL and absorbs gel
Carbon cloth, it is dry under 60 DEG C of air atmospheres.
4) under an ar atmosphere by the treated carbon cloth for absorbing gel, with the heating rate of 5 DEG C/min, 700 DEG C of height
Temperature sintering 10h is dried after respectively washing 3 times with deionized water and ethyl alcohol respectively after natural cooling, obtains final product carbon
Cloth loads LiFePO4Positive electrode.
Fig. 1 is the pure LiFePO of preparation4Carbon cloth prepared by (pristine LFP) sample and the present embodiment 1 loads LiFePO4
(LFP-CC) X-ray diffraction (XRD) of flexible positive electrode compares map, as shown in Figure 1, carbon cloth load manufactured in the present embodiment
LiFePO4Positive electrode has good purity and crystallinity.
Fig. 2 a and Fig. 2 b are that carbon cloth prepared by the embodiment of the present invention 1 loads LiFePO in Fig. 24/ positive electrode scanning electron
Microscope (SEM) map, by Fig. 2 a and Fig. 2 b in Fig. 2 it is found that LiFePO4Active material is equably supported on the carbon fiber of carbon cloth
Surface, active material particle are in monodisperse shape, and particle size is between 50-200 nanometers, it was demonstrated that the preparation method can be effectively
On a flexible substrate by active material load.
Embodiment 2
A kind of self-supporting flexible lithium ion battery carbon cloth of the present embodiment loads LiFePO4The preparation method of positive electrode, packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in deionized water, respectively
Concentration of component is respectively 0.2mol/L, 0.1mol/L, 0.1mol/L and 0.1mol/L, and aqueous solution whole volume is 20mL, and 80 DEG C
Heating stirring forms colloidal sol.
2) carbon cloth is impregnated in above-mentioned colloidal sol, continues 80 DEG C of heating stirring evaporation solvents.
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out when colloidal sol is evaporated to 5mL and absorbs gel
Carbon cloth, it is dry under 60 DEG C of air atmospheres.
4) under an ar atmosphere by the treated carbon cloth for absorbing gel, with the heating rate of 5 DEG C/min, 700 DEG C of height
Temperature sintering 10h is dried after respectively washing 3 times with deionized water and ethyl alcohol respectively after natural cooling, obtains final product carbon
Cloth loads LiFePO4Positive electrode.
Embodiment 3
A kind of self-supporting flexible lithium ion battery carbon cloth of the present embodiment loads LiFePO4The preparation method of positive electrode, packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in deionized water, respectively
Concentration of component is respectively 0.2mol/L, 0.1mol/L, 0.1mol/L, and 0.1mol/L and aqueous solution whole volume are 20mL, and 80 DEG C
Heating stirring forms colloidal sol.
2) carbon cloth is impregnated in above-mentioned colloidal sol, continues 80 DEG C of heating stirring evaporation solvents.
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out when colloidal sol is evaporated to 2mL and absorbs gel
Carbon cloth, it is dry under 60 DEG C of air atmospheres.
4) under an ar atmosphere by the treated carbon cloth for absorbing gel, with the heating rate of 5 DEG C/min, 700 DEG C of height
Temperature sintering 10h is dried after respectively washing 3 times with deionized water and ethyl alcohol respectively after natural cooling, obtains final product carbon
Cloth loads LiFePO4Positive electrode.
Fig. 3 is that carbon cloth prepared by the present embodiment 3 loads LiFePO4The scanning electron microscope (SEM) of flexible positive electrode
Figure.As can be seen from Figure 3 after high concentration dipping, active material is coated on carbon cloth carbon fiber surface, active material layer completely
It is thicker and uniform, it was demonstrated that the preparation method can effectively improve the load capacity of active material on a flexible substrate.
Embodiment 4
A kind of self-supporting flexible lithium ion battery carbon cloth of the present embodiment loads LiFePO4The preparation method of positive electrode, packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in deionized water, respectively
Concentration of component is respectively 0.6mol/L, 0.3mol/L, 0.3mol/L and 0.3mol/L, and aqueous solution whole volume is 20mL, and 60 DEG C
Heating stirring forms colloidal sol.
2) carbon cloth is impregnated in above-mentioned colloidal sol, continues 60 DEG C of heating stirring evaporation solvents.
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out when colloidal sol is evaporated to 1mL and absorbs gel
Carbon cloth, it is dry under 60 DEG C of air atmospheres.
4) under an ar atmosphere by the treated carbon cloth for absorbing gel, with the heating rate of 5 DEG C/min, 600 DEG C of height
Temperature sintering 15h is dried after respectively washing 3 times with deionized water and ethyl alcohol respectively after natural cooling, obtains final product carbon
Cloth loads LiFePO4Positive electrode.
Embodiment 5
A kind of self-supporting flexible lithium ion battery carbon cloth of the present embodiment loads LiFePO4The preparation method of positive electrode, packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in deionized water, respectively
Concentration of component is respectively 1mol/L, 0.5mol/L, 0.5mol/L and 0.5mol/L, and aqueous solution whole volume is 20mL, and 70 DEG C add
Thermal agitation forms colloidal sol.
2) carbon cloth is impregnated in above-mentioned colloidal sol, continues 70 DEG C of heating stirring evaporation solvents.
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out when colloidal sol is evaporated to 5mL and absorbs gel
Carbon cloth, it is dry under 70 DEG C of air atmospheres.
4) under an ar atmosphere by the treated carbon cloth for absorbing gel, with the heating rate of 5 DEG C/min, 800 DEG C of height
Temperature sintering 10h is dried after respectively washing 3 times with deionized water and ethyl alcohol respectively after natural cooling, obtains final product carbon
Cloth loads LiFePO4Positive electrode.
Embodiment 6
A kind of self-supporting flexible lithium ion battery carbon cloth of the present embodiment loads LiFePO4The preparation method of positive electrode, packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in deionized water, respectively
Concentration of component is respectively 0.6mol/L, 0.3mol/L, 0.3mol/L and 0.3mol/L, and aqueous solution whole volume is 20mL, and 80 DEG C
Heating stirring forms colloidal sol.
2) carbon cloth is impregnated in above-mentioned colloidal sol, continues 80 DEG C of heating stirring evaporation solvents.
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, takes out when colloidal sol is evaporated to 2mL and absorbs gel
Carbon cloth, it is dry under 60 DEG C of air atmospheres.
4) under an ar atmosphere by the treated carbon cloth for absorbing gel, with the heating rate of 5 DEG C/min, 900 DEG C of height
Temperature sintering 6h is dried after respectively washing 3 times with deionized water and ethyl alcohol respectively after natural cooling, obtains final product carbon
Cloth loads LiFePO4Positive electrode.
Claims (5)
1. a kind of self-supporting flexible lithium ion battery carbon cloth loads LiFePO4The preparation method of positive electrode, it is characterised in that: packet
Include following steps:
1) monohydrate potassium, lithium nitrate, green vitriol and ammonium dihydrogen phosphate are dissolved in be formed in deionized water and are mixed
Close object, wherein the concentration that monohydrate potassium, lithium nitrate, green vitriol, ammonium dihydrogen phosphate account for mixture is respectively
0.2-1mol/L, 0.1-0.5mol/L, 0.1-0.5mol/L and 0.1-0.5mol/L are heated to 60 DEG C -80 DEG C and stir to be formed
Colloidal sol；
2) carbon cloth is impregnated in above-mentioned colloidal sol, continue to be heated to 60 DEG C -80 DEG C and stirs evaporation solvent；
3) as solvent evaporates, above-mentioned colloidal sol changes to gel process, and the carbon cloth for absorbing gel is taken out in the process different moments,
Obtain different loads amount LiFePO4The carbon cloth composite material of gel, and be dried, the condition that is dried is 60 DEG C -100
It is dry under DEG C air atmosphere；
4) by the treated carbon cloth high temperature sintering under an inert atmosphere for absorbing gel, after washed, ultrasound, it is dry at
Reason obtains final product carbon cloth load LiFePO4Positive electrode, wherein high temperature sintering condition are as follows: be warming up at 600 DEG C -900 DEG C
It is sintered 6-15h, rear natural cooling.
2. a kind of self-supporting flexible lithium ion battery carbon cloth according to claim 1 loads LiFePO4Positive electrode preparation
Method, which is characterized in that the foundation that different moments take out carbon cloth in the step 3) is that colloidal sol is evaporated to the 1/ of original volume respectively
2,1/4,1/10,1/20 when take out carbon cloth.
3. a kind of self-supporting flexible lithium ion battery carbon cloth according to claim 1 loads LiFePO4The preparation of positive electrode
Method, which is characterized in that inert atmosphere is Ar gas atmosphere in the step 4).
4. a kind of self-supporting flexible lithium ion battery carbon cloth according to claim 1 loads LiFePO4The preparation of positive electrode
Method, which is characterized in that heating rate is 5 DEG C/min in step 4) the high temperature sintering condition.
5. a kind of self-supporting flexible lithium ion battery carbon cloth according to claim 1 loads LiFePO4The preparation of positive electrode
Method, which is characterized in that wash conditions are in the step 4): it is respectively washed 3 times with deionized water and ethyl alcohol respectively.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2022145469A (en) * | 2021-03-19 | 2022-10-04 | 積水化学工業株式会社 | Cathode for nonaqueous electrolyte secondary battery, nonaqueous electrolyte secondary battery using the same, battery module, and battery system |
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