CN103840199A - PEO (Polyoxyethylene)-based gel polymer electrolyte membrane, preparation method of membrane, and lithium ion battery - Google Patents
PEO (Polyoxyethylene)-based gel polymer electrolyte membrane, preparation method of membrane, and lithium ion battery Download PDFInfo
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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Abstract
The invention relates to a preparation method of a PEO (Polyoxyethylene)-based gel polymer electrolyte membrane. The preparation method comprises the following steps: (a) preparing a PEO-based gel polymer membrane; and (b) preparing the PEO-based gel polymer electrolyte membrane. The invention also relates to a lithium ion battery assembled through the PEO based gel polymer electrolyte membrane. According to the preparation method, pores are formed in PEO through a pore forming agent, so that the conductivity of the gel polymer electrolyte membrane is effectively improved; after the gel polymer electrolyte membrane is assembled to be the lithium ion battery, the specific capacity of the lithium ion battery can also be improved; in addition, compared with current commercial organic liquid electrolyte, the PEO-based gel polymer electrolyte membrane prepared by adopting the preparation method has the relatively high stability and safety.
Description
Technical field
The present invention relates to electrochemical field, relate in particular to PEO (polyethylene glycol oxide) base gel polymer electrolyte film and preparation method thereof.The invention still further relates to and adopt the prepared lithium ion battery of this PEO base gel polymer electrolyte film.
Background technology
Lithium ion battery is the advantage such as volume is little, lightweight, high power capacity, memory-less effect owing to having, thereby is widely used in the fields such as mobile phone, mobile phone, military affairs and electric automobile.
Lithium-ion battery electrolytes is divided into organic liquid electrolyte and polymer dielectric.The advantage of now widely used liquid electrolyte is that conductivity is high, but inflammable owing to containing, volatile organic solvent, it discharges fuel gas in charge and discharge process, particularly under some unconventional condition of work, (discharge and recharge as high-power, super-charge super-discharge etc.) produces large calorimetric meeting and accelerates the generation of gas, cause inner pressure of battery to increase,, even to blast on fire, thereby there is serious potential safety hazard in Leakage Gas.Polymer electrolyte lithium-ion battery because thering is safety, without leaking, leakage current is little, can arbitrary shape etc. the studied person of advantage pay attention to.Under solid polymer electrolyte room temperature, conductivity is lower by (10
-5~ 10
-4s/cm), use application to be restricted, thereby gel polymer electrolyte (also claiming gel polymer electrolyte film) become research emphasis.
Summary of the invention
The object of the invention is to solve the problem and shortage that above-mentioned prior art exists, a kind of PEO base gel polymer electrolyte film and preparation method thereof and the lithium ion battery that adopts this PEO base gel polymer electrolyte film to assemble are provided.
The technical scheme that the present invention is directed to above-mentioned technical problem and propose is: a kind of preparation method of PEO base gel polymer electrolyte film, comprises the steps.(a) prepare PEO base gelatin polymer film: under inert gas shielding, PEO, organic solvent and pore creating material are stirred 10:30 ~ 50:1 ~ 2 in mass ratio, mix to obtain mucus, be cast in casting film-forming on barrier film, after vacuumize, obtain described PEO base gelatin polymer film; (b) prepare PEO base gel polymer electrolyte film: 10 ~ 60min during dried described PEO base gelatin polymer film is immersed in to lithium salt electrolyte under inert gas shielding, then takes out and obtains PEO base gel polymer electrolyte film.
In described step (a), described organic solvent is chloroform, acetonitrile or carrene; Described pore creating material is ammonium carbonate, carbonic hydroammonium or urea; Described mixing time is 3 ~ 8 hours; Described barrier film is polypropylene non-woven fabric barrier film; Described vacuumize temperature is that 90 ~ 120 ℃, time are 24 ~ 48h.
In described step (b), the concentration of described lithium salt electrolyte is 0.5 ~ 1.5mol/l, the solute of described lithium salt electrolyte is that lithium hexafluoro phosphate, solvent are ethylene carbonate and dimethyl carbonate, and wherein, the volume ratio of ethylene carbonate and dimethyl carbonate is 1:1 ~ 2.
The present invention also comprises the PEO base gel polymer electrolyte film that utilizes above-mentioned preparation method to make.
Above-mentioned PEO base gel polymer electrolyte film can be assembled into lithium ion battery, this lithium ion battery comprises the dielectric film between positive electrode, negative electrode and described positive and negative electrode, described positive electrode comprises collector and is coated in this collector spreading mass, described dielectric film is above-mentioned PEO base gel polymer electrolyte film, described slurry by LiFePO4, acetylene black, Kynoar, 1-METHYLPYRROLIDONE in mass ratio 9:0.45:0.45:20 be uniformly mixed and form.
The present invention decomposes by pore creating material ammonium carbonate, carbonic hydroammonium or urea gases such as producing carbon dioxide, ammonia in the dry run of 90～120 ℃, these gases play the effect of pore-creating and form the gel-type polymer electrolyte film of loose structure in PEO, the gel-type polymer electrolyte film of this loose structure is more conducive to adsorb electrolyte, thereby improves conductivity.
The transfer function that the existing polymer segment of electrical conduction mechanism of gel-type polymer electrolyte film moves to lithium ion, has again the migration in the liquid microfacies that lithium ion provides at plasticizer.
The advantage of the prepared PEO base gel polymer electrolyte film of the present invention is: 1, the present invention is by pore creating material pore-creating on PEO, can effectively improve the conductivity of gel polymer electrolyte film, this gel polymer electrolyte film is assembled into after lithium ion battery, and the specific capacity of lithium ion battery is also improved.2, the PEO base gel polymer electrolyte film that prepared by the present invention and current commercial liquid organic electrolyte (inflammable, volatile, thermal stability is bad etc.) are compared has good stability and fail safe.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.Following examples are for the present invention is described, to instruct those skilled in the art to realize the present invention, the present embodiment does not limit the present invention in any way.
The preparation process that the present invention prepares PEO base gel polymer electrolyte film (hereinafter to be referred as gel polymer electrolyte film) is roughly divided into following two steps.(a) prepare PEO base gelatin polymer film: 10:30 ~ 50:1 ~ 2 add respectively PEO, organic solvent and pore creating material in mass ratio in flask, and under inert gas shielding, stir 3-8h and make it mix the liquid that obtains thickness.Then, acquisition is cast in to PP(polypropylene) casting film-forming on nonwoven fabrics barrier film, and vacuum degree is 0.01MPa vacuumize 24-48h at 90-120 ℃.In the dry run of 90-120 ℃, pore creating material decomposes gases such as producing carbon dioxide, ammonia and plays the effect of pore-creating, thereby obtains described PEO base gelatin polymer film.(b) prepare PEO base gel polymer electrolyte film: dried described PEO base gelatin polymer film is put in the glove box that is full of argon gas, and be immersed in 10 ~ 60min in lithium salt electrolyte, then take out and obtain PEO base gel polymer electrolyte film.
In described step (a), described organic solvent is chloroform, acetonitrile or carrene; Described pore creating material is ammonium carbonate, carbonic hydroammonium or urea.
In described step (b), the concentration of described lithium salt electrolyte is 0.5 ~ 1.5mol/l, and in described lithium salt electrolyte, solute is lithium hexafluoro phosphate (LiPF
6), solvent is ethylene carbonate (EC) and dimethyl carbonate (DMC), also can be abbreviated as LiPF
6same under/EC+DMC(), wherein, EC+DMC represents ethylene carbonate (EC) and dimethyl carbonate (DMC) mixed solvent, volume ratio is 1:1 ~ 2, also can be abbreviated as volume ratio 1:1 ~ 2 of EC:DMC, lower same.
The present invention also comprises and utilizes above-mentioned preparation method to make PEO base gel polymer electrolyte film.
Above-mentioned PEO base gel polymer electrolyte film can be assembled into lithium ion battery, this lithium ion battery comprises the dielectric film between positive electrode, negative electrode and described positive and negative electrode, described positive electrode comprises collector and is coated in this collector spreading mass, and described dielectric film is above-mentioned PEO base gel polymer electrolyte film.
Described slurry by LiFePO4, acetylene black, Kynoar, 1-METHYLPYRROLIDONE in mass ratio 9:0.45:0.45:20 be uniformly mixed and form.
The preparation method of described lithium ion battery is: 9:0.45:0.45:20 gets LiFePO4, acetylene black, Kynoar, 1-METHYLPYRROLIDONE and fully stirs and make it to become the slurry mixing in mass ratio.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 80 ° of C are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into electrode film (be also described positive electrode, lower with).Lithium sheet is negative electrode.PEO base gel polymer electrolyte film of the present invention is placed between described positive and negative electrode, and on stamping machine, fastening lithium ionic cell is made in sealing.
Below with 1 ~ 4 pair of PEO base gel polymer electrolyte film of the present invention of embodiment and apply the preparation method that this gel polymer electrolyte film is assembled into lithium ion battery and be specifically described.
embodiment 1
In the embodiment of the present invention 1, the preparation method of gel polymer electrolyte film comprises the steps.(a) prepare PEO base gelatin polymer film: in flask, add respectively 10gPEO, 40g chloroform and 1.5g ammonium carbonate, and under inert gas shielding, stir 6h and make it mix the liquid that obtains thickness.Then, acquisition mucus is cast in to casting film-forming on polypropylene non-woven fabric barrier film, and vacuum degree is 0.01MPa vacuumize 30h at 100 ℃, thereby obtains described PEO base gelatin polymer film.(b) prepare PEO base gel polymer electrolyte film: the PEO base gelatin polymer film transfer that step (a) is prepared is to being full of in the glove box of argon gas, and immersed the LiPF of 1.2mol/L
6the volume ratio 1:1 of/EC+DMC(EC:DMC) middle 30min.Taken out and obtained PEO base gel polymer electrolyte film.
The preparation method that the above-mentioned PEO base gel polymer electrolyte film making is assembled into lithium ion battery is: take 9.0g LiFePO4,0.45g acetylene black, 0.45g Kynoar, 20gN-methyl pyrrolidone and fully stir and make it to become the slurry mixing.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 80 ° of C are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into electrode film.Lithium sheet is negative electrode.Above-mentioned PEO base gel polymer electrolyte film is placed between described positive and negative electrode, and on stamping machine, fastening lithium ionic cell is made in sealing.
embodiment 2
In the embodiment of the present invention 2, the preparation method of gel polymer electrolyte film comprises the steps.(a) prepare PEO base gelatin polymer film: in flask, add respectively 10gPEO, 30g acetonitrile and 1.0g carbonic hydroammonium, and under inert gas shielding, stir 8h and make it mix the liquid that obtains thickness.Then, acquisition mucus is cast in to casting film-forming on polypropylene non-woven fabric barrier film, and vacuum degree is 0.01MPa vacuumize 48h at 90 ℃, thereby obtains described PEO base gelatin polymer film.(b) prepare PEO base gel polymer electrolyte film: the PEO base gelatin polymer film transfer that step (a) is prepared is to being full of in the glove box of argon gas, and immersed the LiPF of 0.5mol/L
6the volume ratio 1:2 of/EC+DMC(EC:DMC) middle 60min.Taken out and obtained PEO base gel polymer electrolyte film.
The preparation method that the above-mentioned PEO base gel polymer electrolyte film making is assembled into lithium ion battery is: take 9.0g LiFePO4,0.45g acetylene black, 0.45g Kynoar, 20gN-methyl pyrrolidone and fully stir and make it to become the slurry mixing.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 80 ° of C are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into electrode film.Lithium sheet is negative electrode.Above-mentioned PEO base gel polymer electrolyte film is placed between described positive and negative electrode, and on stamping machine, fastening lithium ionic cell is made in sealing.
embodiment 3
In the embodiment of the present invention 3, the preparation method of gel polymer electrolyte film comprises the steps.(a) prepare PEO base gelatin polymer film: in flask, add respectively 10gPEO, 50g carrene and 2.0g urea, and under inert gas shielding, stir 3h and make it mix the liquid that obtains thickness.Then, acquisition mucus is cast in to casting film-forming on polypropylene non-woven fabric barrier film, and vacuum degree is 0.01MPa vacuumize 24h at 120 ℃, thereby obtains described PEO base gelatin polymer film.(b) prepare PEO base gel polymer electrolyte film: the PEO base gelatin polymer film transfer that step (a) is prepared is to being full of in the glove box of argon gas, and immersed the LiPF of 1.5mol/L
6the volume ratio 1:1 of/EC+DMC(EC:DMC) middle 10min.Taken out and obtained PEO base gel polymer electrolyte film.
The preparation method that the above-mentioned PEO base gel polymer electrolyte film making is assembled into lithium ion battery is: take 9.0g LiFePO4,0.45g acetylene black, 0.45g Kynoar, 20gN-methyl pyrrolidone and fully stir and make it to become the slurry mixing.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 80 ° of C are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into electrode film.Lithium sheet is negative electrode.Above-mentioned PEO base gel polymer electrolyte film is placed between described positive and negative electrode, and on stamping machine, fastening lithium ionic cell is made in sealing.
embodiment 4
In the embodiment of the present invention 1, the preparation method of gel polymer electrolyte film comprises the steps.(a) prepare PEO base gelatin polymer film: in flask, add respectively 10gPEO, 45 acetonitriles and 1.7g urea, and under inert gas shielding, stir 6h and make it mix the liquid that obtains thickness.Then, acquisition mucus is cast in to casting film-forming on polypropylene non-woven fabric barrier film, and vacuum degree is 0.01MPa vacuumize 36h at 110 ℃, thereby obtains described PEO base gelatin polymer film.(b) prepare PEO base gel polymer electrolyte film: the PEO base gelatin polymer film transfer that step (a) is prepared is to being full of in the glove box of argon gas, and immersed the LiPF of 0.9mol/L
6the volume ratio 1:2 of/EC+DMC(EC:DMC) middle 30min.Taken out and obtained PEO base gel polymer electrolyte film.
The preparation method that the above-mentioned PEO base gel polymer electrolyte film making is assembled into lithium ion battery is: take 9.0g LiFePO4,0.45g acetylene black, 0.45g Kynoar, 20gN-methyl pyrrolidone and fully stir and make it to become the slurry mixing.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 80 ° of C are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into electrode film.Lithium sheet is negative electrode.Above-mentioned PEO base gel polymer electrolyte film is placed between described positive and negative electrode, and on stamping machine, fastening lithium ionic cell is made in sealing.
comparative example
The preparation method of comparative example PEO base gel polymer electrolyte film of the present invention comprises the steps.(a) prepare PEO base gelatin polymer film: in flask, add respectively 10gPEO, 40g acetonitrile, and under inert gas shielding, stir 6h and make it mix the liquid that obtains thickness.Then, acquisition mucus is cast in to casting film-forming on polypropylene non-woven fabric barrier film, and vacuum degree is 0.01MPa vacuumize 36h at 100 ℃, thereby obtains PEO base gelatin polymer film.Be not add pore creating material with the difference of above-described embodiment.(b) prepare PEO base gel polymer electrolyte film: the PEO base gelatin polymer film transfer that step (a) is prepared is to being full of in the glove box of argon gas, and immersed the LiPF of 1.2mol/L
6the volume ratio 1:1 of/EC+DMC(EC:DMC) middle 30min.Taken out and obtained PEO base gel polymer electrolyte film.
The preparation method that the above-mentioned PEO base gel polymer electrolyte film making is assembled into lithium ion battery is: take 9.0g LiFePO4,0.45g acetylene black, 0.45g Kynoar, 20gN-methyl pyrrolidone and fully stir and make it to become the slurry mixing.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 80 ° of C are dried to constant weight, and are pressed into iron phosphate lithium electrode in 10 ~ 15MPa pressure lower roll, and are cut into electrode film.Lithium sheet is negative electrode.Above-mentioned PEO base gel polymer electrolyte film is placed between described positive and negative electrode, and on stamping machine, fastening lithium ionic cell is made in sealing.
The method of testing of the conductivity of prepared PEO base gel polymer electrolyte film is:
Between two stainless steel blocking electrodes, add the PEO base gel polymer electrolyte film preparing, form the electrode system that polymer dielectric film blocks, do ac impedance measurement, obtain the complex impedance plane graph of GPE.The curve of described figure is the body impedance of described PEO base gel polymer electrolyte film in the intersection value of high frequency region and transverse axis.According to the body impedance (R of described PEO base gel polymer electrolyte film
b) and its conductivity (σ) between relation:
σ=d/(S*?R
b)
Can calculate the conductivity (σ) of described PEO base gel polymer electrolyte film, wherein d is that thickness, the S of described PEO base gel polymer electrolyte film are the contact area of described PEO base gel polymer electrolyte film and described stainless steel blocking electrode.The conductivity that table 1 is PEO base gel polymer electrolyte film prepared in the present embodiment and the lithium ion battery assembling carry out the performance data of 0.2C charge-discharge test in 2.5～4.2 voltage range by charge-discharge test instrument.
Table 1
| Table 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example |
| The conductivity ms/cm of prepared PEO base gel polymer electrolyte film | 4.2 | 2.7 | 3.5 | 3.8 | 1.2 |
| The lithium ion battery first discharge specific capacity mAh/g assembling | 116 | 100 | 107 | 112 | 92 |
As can be seen from Table 1, the conductivity of the PEO base gel polymer electrolyte film preparing by embodiment 1 ~ 4 method is greater than the conductivity of comparative example, and reaches 4.2ms/cm in embodiment 1; The first discharge specific capacity of the lithium ion battery assembling by embodiment 1 ~ 4 method is all greater than the specific capacity in comparative example, and has arrived 116mAh/g than electric capacity in embodiment 1.
Can draw such conclusion from above data, the present invention is by pore creating material pore-creating on PEO, the conductivity that can effectively improve gel polymer electrolyte film, is assembled into this gel polymer electrolyte film after lithium ion battery, and the specific capacity of lithium ion battery is also improved.
Foregoing; it is only preferred embodiment of the present invention; not for limiting embodiment of the present invention; those of ordinary skills are according to main design of the present invention and spirit; can carry out very easily corresponding flexible or modification, therefore protection scope of the present invention should be as the criterion with the desired protection range of claims.
Claims (10)
1. a preparation method for PEO base gel polymer electrolyte film, is characterized in that, comprises the steps:
(a) prepare PEO base gelatin polymer film: under inert gas shielding, PEO, organic solvent and pore creating material are stirred 10:30 ~ 50:1 ~ 2 in mass ratio, mix to obtain mucus, be cast in casting film-forming on barrier film, after vacuumize, obtain described PEO base gelatin polymer film;
(b) prepare PEO base gel polymer electrolyte film: 10 ~ 60min during dried described PEO base gelatin polymer film is immersed in to lithium salt electrolyte under inert gas shielding, then takes out and obtains PEO base gel polymer electrolyte film.
2. preparation method according to claim 1, is characterized in that, in described step (a), described organic solvent is chloroform, carrene or acetonitrile.
3. preparation method according to claim 1, is characterized in that, in described step (a), described pore creating material is ammonium carbonate, carbonic hydroammonium or urea.
4. preparation method according to claim 1, is characterized in that, in described step (a), described mixing time is 3 ~ 8 hours.
5. preparation method according to claim 1, is characterized in that, in described step (a), described barrier film is polypropylene non-woven fabric barrier film.
6. preparation method according to claim 1, is characterized in that, in described step (a), described vacuumize temperature is that 90 ~ 120 ℃, time are 24 ~ 48h.
7. preparation method according to claim 1, it is characterized in that, in described step (b), the concentration of described lithium salt electrolyte is 0.5 ~ 1.5mol/l, the solute of described lithium salt electrolyte is that lithium hexafluoro phosphate, solvent are ethylene carbonate and dimethyl carbonate, wherein, the volume ratio of ethylene carbonate and dimethyl carbonate is 1:1 ~ 2.
8. the PEO base gel polymer electrolyte film that the arbitrary described preparation method of claim 1 to 7 makes.
9. a lithium ion battery, comprise the dielectric film between positive electrode, negative electrode and described positive and negative electrode, described positive electrode comprises collector and is coated in this collector spreading mass, it is characterized in that, described dielectric film is PEO base gel polymer electrolyte film claimed in claim 8.
10. lithium ion battery according to claim 9, is characterized in that, described slurry by LiFePO4, acetylene black, Kynoar, 1-METHYLPYRROLIDONE in mass ratio 9:0.45:0.45:20 be uniformly mixed and form.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106785030A (en) * | 2016-12-27 | 2017-05-31 | 深圳市星源材质科技股份有限公司 | A kind of preparation method of full solid state polymer electrolyte |
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| CN101577350A (en) * | 2009-06-04 | 2009-11-11 | 浙江大学 | Gel polymer electrolyte with semi-interpenetrating network structure and preparation method thereof |
| CN102286158A (en) * | 2011-06-23 | 2011-12-21 | 中南大学 | Method for preparing porous composite polymer electrolyte film through gas volatilization |
| CN102610857A (en) * | 2012-03-01 | 2012-07-25 | 合肥国轩高科动力能源有限公司 | Method for preparing polyoxyethylene gel polymer electrolyte membrane |
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| CN101440188A (en) * | 2008-12-30 | 2009-05-27 | 哈尔滨工业大学 | Lithium ionic cell gel type ion liquid / polymer electrolyte and preparation thereof |
| CN101577350A (en) * | 2009-06-04 | 2009-11-11 | 浙江大学 | Gel polymer electrolyte with semi-interpenetrating network structure and preparation method thereof |
| CN102286158A (en) * | 2011-06-23 | 2011-12-21 | 中南大学 | Method for preparing porous composite polymer electrolyte film through gas volatilization |
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| CN106785030A (en) * | 2016-12-27 | 2017-05-31 | 深圳市星源材质科技股份有限公司 | A kind of preparation method of full solid state polymer electrolyte |
| CN106785030B (en) * | 2016-12-27 | 2020-08-25 | 深圳市星源材质科技股份有限公司 | Preparation method of all-solid-state polymer electrolyte |
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Application publication date: 20140604 |